By Authority Of
THE UNITED STATES OF AMERICA
Legally Binding Document
By the Authority Vested By Part 5 of the United Stat...
OFFICIAL
METHODS OF ANALYSIS
OF THE
ASSOCIATION OF OFFICIAL
ANALYTICAL CHEMISTS
WILLIAM HORWITZ, Editor
THIRTEENTH EDITION...
Direct inquiries related to the scientific content of Official Methods of Analysis to:
Editor, Official Methods of Analysi...
Preface to Thirteenth Edition
The most noticeable physical change in this thirteenth edition
of Official Methods of Analys...
effectiveness in identifying Salmonella and other enteric isolates.
A criticism that is often leveled at the AOAC validati...
Contents
Preface to Thirteenth Edition ......................... .
Preface to First Edition .................................
PAGE
Dithiocarbamates . . . . . . . . . . . . . . . . . . . . . .. . . . . . 110
Thiram ............................... '"...
PAGE PAGE
Lemon Juice .................................. 372 Carbaryl .................................... 483
Sulphenone ...
PAGE
Inorganic Drugs ............................... 594
Mydriatics and Myotics ........................ 604
Microscopic T...
FIGURE
1:01.
2:01.
2:02.
2:03.
2:04.
2:05.
2:06.
2:07.
2:08.
3:01.
3:02.
3:03.
3:04.
3:05.
3:06.
3:07.
4:01.
4:02.
6:01.
6...
FIGURE PAGE
18:03. Muscle Bath ..............................................................................................
FIGURE PAGE
37:02. Flow Diagram for Automated Analysis for Acenocoumarol, Dicumarol, Phenprocoumon, Potassium Warfarin, an...
Collaborative Study Procedures of the Association of
Official Analytical Chemists
The Association of Official Analytical C...
In clinical chemistry, within-laboratory precision (repeatability)
is critical, and often is of greater interest to clinic...
is emphasized beforehand and the participants provide a de-
scription of the method used in order to permit a correlation ...
Definitions of Terms and Explanatory Notes
Reagents
(1) Term "H20" means distilled water, except where otherwise
specified...
(21) Unless otherwise indicated, temps are expressed as
degrees Centigrade.
Table 1. Nominal Dimensions of Standard Test S...
Many scientific and statistical calculators are preprogrammed
to perform this calcn.
(25) Common safety precautions are gi...
Schoeffellnstrument Corp., 24 Booker St, Westwood, NJ 07675
SGA Scientific, Inc., 735 Broad St, Bloomfield, NJ 07003
Scien...
Abbreviation
detg
detn
diam.
diat. earth
dil.
dild
dilg
diln
distd
distg
distn
DMF
DMSO
EDTA
e.g.
elec.
equiv.
est.
estd
e...
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Aoac.methods.1980
Upcoming SlideShare
Loading in...5
×

Aoac.methods.1980

3,982

Published on

Relação de metodologias para análises de alimentos

Published in: Food, Technology
1 Comment
3 Likes
Statistics
Notes
  • Great presentation. Thanks for the info. Does anyone know where I can find a blank usda form rd 1980 21 to fill out?
       Reply 
    Are you sure you want to  Yes  No
    Your message goes here
No Downloads
Views
Total Views
3,982
On Slideshare
0
From Embeds
0
Number of Embeds
0
Actions
Shares
0
Downloads
328
Comments
1
Likes
3
Embeds 0
No embeds

No notes for slide

Transcript of "Aoac.methods.1980"

  1. 1. By Authority Of THE UNITED STATES OF AMERICA Legally Binding Document By the Authority Vested By Part 5 of the United States Code § 552(a) and Part 1 of the Code of Regulations § 51 the attached document has been duly INCORPORATED BY REFERENCE and shall be considered legally binding upon all citizens and residents of the United States of America. HEED THIS NOTICE: Criminal penalties may apply for noncompliance. Official Incorporator: THE EXECUTIVE DIRECTOR OFFICE OF THE FEDERAL REGISTER WASHINGTON, D.C. Document Name: CFR Section(s): Standards Body: e AOAC: Official Methods of Analysis, 1980 21 CFR 131.150(c) AOAC International
  2. 2. OFFICIAL METHODS OF ANALYSIS OF THE ASSOCIATION OF OFFICIAL ANALYTICAL CHEMISTS WILLIAM HORWITZ, Editor THIRTEENTH EDITION, 1980 PUBLISHED BY THE ASSOCIATION OF OFFICIAL ANALYTICAL CHEMISTS PO Box 540, BENJAMIN FRANKLIN STATION WASHINGTON, DC 20044
  3. 3. Direct inquiries related to the scientific content of Official Methods of Analysis to: Editor, Official Methods of Analysis Association of Official Analytical Chemists Box 540, Benjamin Franklin Station Washington, DC 20044 USA Direct inquiries related to the procurement of Official Methods of Analysis, supplements (Changes in Methods). Journal of the AOAC, or other AOAC publications to: Assistant Business Manager, Publications Association of Official Analytical Chemists 1111 N 19th Street (Suite 210) Arlington, VA 22209 USA (Telephone: 703-522-3032) COPYRIGHT 1920,1925, 1931, 1936, 1940, 1945, 1950, 1955, 1960, 1965, BYTHE ASSOCIATION OF OFFICIAL AGRICULTURAL CHEMISTS AND 1970, 1975, 1980 BY THE ASSOCIATION OF OFFICIAL ANALYTICAL CHEMISTS The methods of the Association were also copyrighted in 1916, when they were published in the Journal of the Association of Official Agricultural Chemists Library of Congress Catalog Card Number: 20-21343 ISBN 0-935584-14-5 A copy of the 13th edition of this publication is on file with the Office of the Federal Register. U. S. Government Agencies may apply to the Director of the Office of the Federal Register for approval to incorporate this edition by reference in their regulations. The procedures that Federal agencies must follow in applying for the Director's approval are in Title 1, Part 51 of the Code of Federal Regulations. Composed by Monotype Composition Company, Inc. Baltimore, Maryland Printed and bound by George Banta Company, Inc. Menasha, Wisconsin ii
  4. 4. Preface to Thirteenth Edition The most noticeable physical change in this thirteenth edition of Official Methods of Analysis of the Association of Official Analytical Chemists ("The Book of Methods") is its size. A survey of users of the Book of Methods revealed an overwhelming desire to maintain the compendium as a single volume. The easiest way to do this was to increase the size of the page. Users also expressed a desire for a system that will keep the same reference number for a given method from edition to edition. A practical system that will maintain the continuity of the numbering system and the organizational structure of the methods within a chapter has not yet been devised. Approximately 175 new methods have been added during the current five year period (1974-1978); 83 methods have been deleted, replaced, or surplused. The approval of an average of only 35 new methods per year represents a marked decline from the 70 per year of the four year period of the previous edition (1970-1973) and the 50 per year of the five year period of the tenth edition (1965-1969). The decline is undoubtedly the result of a number of factors. Chief among them are the greater complexity of modern methods, requiring a large investment in resources that is not readily mobilized to fit an Associate Referee's schedule; and the fact that government agencies are attempting to obtain compliance, especially of the newer stat- utes, by promulgation of regulations and by auditing rather than by laboratory examinations. The greatest activity, as measured by approval of new meth- ods, is in the field of pesticide formulations, partly as a result of the active implementation of the cooperative agreement with the Collaborative International Pesticide Analytical Council (CIPAC). Other active areas include extraneous materials, vita- mins and other nutrients, dairy products, and microbiological methods. In fact, examination for and by biological constituents (filth, microbiological assays, and examination for food-borne pathogens) comprises approximately 17% of the new methods adopted. A comparison of the types of methods adopted between this and the previous edition reveals that gas-liquid chromatography has overtaken spectrophotometry in its various forms (visible, ultraviolet, and fluorescent) as the most predominant quanti- tative technique in Official Methods. High pressure (or perform- ance) liquid chromatography has spurted from none to 6% of the adopted methods within the relatively short period of five years. Electrometric methods (potentiometric, polarographic, and ion-selective) are now sufficiently numerous to deserve a separate category. Infrared methods are no longer a major factor in quantitation; they are now mainly used for identification and confirmation. A comparison of the present and previous editions is presented in Table 1. The figures given are only rough approximations because of the arbitrariness often re- quired in classifying a method and in deciding when a new method or revision is sufficiently independent to warrant con- tributing to the statistics. iii Table 1. Classification of new methods approved by the AOAC in the thirteenth and twelfth editions Method classification Gas-liquid chromatography Spectrophotometry Titrimetric Filth, isolation Automated Biological and microbiological High pressure liquid chromatography Atomic absorption Electrometric Chromatography (thin layer, etc.) Gravimetric Miscellaneous (physical, qualitative, etc.) 13th edition (1980) 18% 16 10 8 7 9 6 4 5 3 2 11 12th edition (1975) 14% 20 7 14 5 8 9 3 6 13 The most interesting new collaboratively studied method is the mass spectrometric method for the detection of adulteration of honey with high fructose corn sirup. Corn sirups (from a monocotyledonous plant) have a distinctly different 13C/12 C ratio than sirups from most dicotyledonous plants, which are the source of most honeys. The isotope ratio mass spectrometer required forthis determination is a highly specialized instrument, even in the field of mass spectrometry. Despite the rarity of the instrumentation, sufficient laboratories participated in the col- laborative study to establish the reproducibility of the method. A problem that has arisen is how to handle the numerous individual instruments of diverse design and manufacture that have been developed to automate a particular determination. Even if this problem is solved by incorporating all the available instruments into the initial collaborative study, the problem returns with the first "new and improved" modification. Different instrument designs and their subsequent modifications have been handled in the infrared determination of milk constituents by providing performance specifications which must be met by the basic instrument in general, when compared to a reference method or reference sample. In addition, the user must satisfy himself that his particular instrument also meets the perform- ance specifications by frequent comparisons with the reference method or sample. This requirement eliminates the need for repeated collaborative studies every time a manufacturer rede- signs or modifies his basic equipment, and in addition provides a continuous quality control technique on the performance of the instrument, method, and laboratory. It should not be overlooked that automation is not confined to physical and chemical determinations. The microbiological chapter contains three collaboratively studied instrumental methods for somatic cell count and an instrumental method for distributing a liquid sample for plate counting. Biochemical diagnostic kits have also been evaluated collaboratively for their
  5. 5. effectiveness in identifying Salmonella and other enteric isolates. A criticism that is often leveled at the AOAC validation mechanism is that it is too slow to keep up with the pace of requirements for methods by regulatory agencies and the regulated industry. This objection overlooks the point that the speed with which a method is validated is almost completely in the hands of those needing the validated method, rather than in the hands of the AOAC. The method must be tested for ruggedness, and the directions tested for clarity; samples must be prepared and distributed; laboratories must analyze the samples and report the results. Dubious results must be inves- tigated and occasionally samples must be reanalyzed. The data must be tabulated and analyzed, and a report written. There is no way to short-cut the process of obtaining intra- and interlab- oratory variability except to conduct the necessary experimental work and perform the necessary statistical calculations. Only then is the recommendation subject to the time restrictions of the AOAC mechanism. To ensure that the AOAC mechanism of annual approval is not holding up use of needed methods, a new temporary class of methods has been introduced entitled "Interim First Action." These are methods which, together with their supporting studies, have been received between annual meetings and have been sent through the customary reviewing procedure. To be designated Interim First Action, a method must have been approved by the appropriate Referee and Subcommittee, and by the Chairman of the Committee on Official Methods. The method only lacks the formal vote by those AOAC members having regulatory authority over the commodity involved. Such formal approval is usually provided at the next annual meeting, at which time the method becomes "First Action." Approximately five interim methods are approved annually. Several such methods appear in this volume, depend- ing upon the time of their submission and review in relation to the editorial status of the chapter to which they are assigned. The current status of these Interim First Action methods, as well as the status of any method, can be found by consulting the latest cumulative index to Changes in Methods, which appears as the final pages of each March issue of the Journal. For those users of AOAC methods who may not be familiar with the procedures by which a method is included in this volume, we are reprinting a paper prepared for the Joint International Symposium, "The Harmonization of Collaborative Studies," held in London, England 9-10 March 1978. The document was drafted by the AOAC Committee on Collaborative Studies: Elwyn D. Schall, Chairman; Charles W. Gehrke, William Horwitz, Anthony J. Malonski, James P. Minyard, Jr., Forrest W. Quackenbush, and Ernest S. Windham. This paper appeared in Analytical Chemistry (March 1978), 50, 337A-340A. The publication of this "Book of Methods" is possible only because of the extensive cooperation of thousands of analysts who have volunteered to direct, participate in, and review the numerous collaborative studies that form the basis for inclusion of the several thousand methods that appear herein. Special recognition is due to Mrs. Betty Johnson who has prepared an entirely new index for this edition. 28 September, 1979 William Horwitz, Ph.D. Editor Abstract from Preface to First Edition "In presenting this revision of the official and tentative methods of analysis of the Association of Official Agricultural Chemists, it is appropriate to give a brief statement of the organization of the Association, its purpose, and the procedure by which the methods are adopted. "Membership in the Association is institutional and includes the State Departments of Agriculture, the State Agricultural Colleges and Experiment Stations, the Federal Department of Agriculture, and the Federal, State, and City offices charged with the enforcement of food, feed, drug, fertilizer, insecticide and fungicide control laws. "The Association was founded at Philadelphia, Pa., September 9, 1884, by the following representative agricultural chemists of that time, the organization being the result of a series of informal meetings held the immediately preceding years: "Prof. H. W. Wiley, Chemist of the Department of Agriculture, Washington, D.C. Mr. Clifford Richardson, Assistant Chemist of the Department of Agriculture, Washington, D.C. Mr. Philip E. Chazal, State Chemist of South Carolina. Dr. Chas. W. Dabney, Jr., State Chemist of North Carolina. Dr. W. J. Gascoyne, State Chemist of Virginia. Dr. E. H. Jenkins, Connecticut Experiment Station. Prof. John A. Meyers, State Chemist of Mississippi. Prof. H. C. White, State Chemist of Georgia. Mr. C. DeGhequier, Secretary National Fertilizer Association. Dr. Schumann, Dr. Lehmann, Mr. Gaines and others." iv
  6. 6. Contents Preface to Thirteenth Edition ......................... . Preface to First Edition .............................. . List of Illustrations .................................. . Collaborative Study Procedures of the Association of Official Analytical Chemists ........................ . Definitions of Terms and Explanatory Notes .......... . CHAPTER 1. Agricultural Liming Materials .................... . Calcium Silicate Slags ........................ . Elemental Analysis ........................... . 2. Fertilizers ....................................... . Free Water ................................... . Phosphorus .................................. . Nitrogen ..................................... . Potassium ................................... . Other Elements ............................... . Peat ......................................... . 3. Plants .......................................... . Metals ....................................... . Nonmetals ................................... . Other Constituents ........................... . Pigments .................................... . Tobacco ..................................... . 4. Disinfectants .................................... . Phenol Coefficient ............................ . Use-Dilution Method .......................... . Available Chlorine Germicidal Equivalent Concentration .............................. . Sporicidal Test ............................... . Fungicidal Test ............................... . Germicidal and Detergent Sanitizers ........... . Germicidal Spray Products .................... . Water Disinfectants for Swimming Pools ....... . Tuberculocidal Activity ........................ . Bacteriostatic Activity of Laundry Additives .... . 5. Hazardous Substances .......................... . Paint ......................................... . Preparations Containing Fluorides ............. . Preparations Containing Methanol ............. . Preparations Containing Phenol ............... . Soda Lye .................................... . Earthenware ................................. . 6. Pesticide Formulations .......................... . General Methods ............................. . Arsenic .................................... . Lead ....................................... . Copper .................................... . Zinc ....................................... . Fluorine .................................... . PAGE iii iv ix xii xv 2 3 7 9 9 14 18 20 27 31 31 38 46 49 51 56 56 58 59 60 61 61 63 64 ' 65 67 69 69 69 70 71 71 71 72 72 72 74 74 75 75 v Contamination by Organochlorine Pesticides .. Volatility of Ester Forms of Hormone-Type Herbicides ............................... . Inorganic and Organometallic Pesticides and Adjuvants ................................ . Paris Green ................................ . Lead Arsenate .............................. . PAGE 77 77 78 78 78 Calcium Arsenate. . . . . . . . . . . . . . . . . . . . . . . . . . . . 79 Zinc Arsenite. . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . 79 Copper Carbonate .. . . . . . . . . . . . . . . . . . . . . . . . . . 79 Copper Naphthenate . . . . . . . . . . . . . . . . . . . . . . . . . 79 Bordeaux Mixtures .......................... 80 Potassium Cyanate. . . . . . . . . . . . . . . . . . . . . . . . . . 81 Cyanides. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 81 Lime Sulfur Preparations. . . . . . . . . . . . . . . . . . . . . 81 Hypochlorites ............................... 82 Chloramine T ............................... 83 Mineral Oils. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 83 Soap....................................... 83 Mineral Oil-Soap Emulsions. . . . . . . . . . . . . . .. . . 83 Mercurial Seed Disinfectants. . . . . . . . . . . . . .. . . 84 Ant Poisons and Rodenticides . . . . . . . . . . . . . . . . 85 Fumigants .................................. 85 Pesticides Related to Natural Products and Their Synergists ................................ 86 Allethrin .................................... 86 Derris and Cube Powder. . . . . . . . . . . . . . . . . .. . . 87 Pyrethrins . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . 89 Tobacco and Tobacco Products .............. 90 Halogenated Pesticides ........................ 91 Aldrin, Dieldrin, and Endrin .................. 91 Amiben ..................................... 93 BHC ........................................ 93 Balan or Trifluralin .......................... 95 Captan . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 96 Chlordane. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 97 Chlorotoluron, Chloroxuron, or Metoxuron . . . . 99 Dichlobenil .. . . .. . ... . . . .. .. . .. . . ... . . . .. ... . 100 DDT.. . . . ... . . ..... . .. . . . .. . ... . . . . .. . .... . . 100 Dacthal ..................................... 102 Dicamba .................................... 102 2,4-D ....................................... 103 Dalapon .................................... 104 Dicofol . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 104 Fluometuron ................................ 105 Folpet ...................................... 105 Heptachlor . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 105 Picloram-2,4-D .............................. 106 Sodium Trichloroacetate ......... " .. . . .... .. 107 Nonhalogenated Pesticides .................... 107 Aldicarb .................................... 107 Amitrole .................................... 107 Carbaryl .................................... 108 DDVP ................... '" ..... " . . ... . .. . . 108 Diquat and Paraquat ............. " . . . . . . . . . . 109
  7. 7. PAGE Dithiocarbamates . . . . . . . . . . . . . . . . . . . . . .. . . . . . 110 Thiram ............................... '" . ... 111 Dodine...................................... 111 Formaldehyde. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 111 Ethion ...................................... 112 Formothion ................................. 113 Malathion. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 113 Parathion ................................... 116 Phorate ... . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 119 Sulfoxide ................................... 120 Tetraethylpyrophosphate .................... 120 Organic Thiocyanates . . . . . . . . . . . . . . . . . . . . . . . . 120 Thiocarbamates ............................. 121 Triazines, Diazinon, and Dichlorobenzilates . . . . 121 Triphenyltin Compounds. . . . . . .. . . . . . . .. . . . . . 122 Quaternary Ammonium Compounds ........... 123 7. Animal Feed..................................... 125 Nitrogen ...................................... 125 Other Constituents ............................ 132 Preservatives. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 141 8. Baking Powders and Baking Chemicals ........... . 9. Beverages: Distilled Liquors ..................... . Spirits ....................................... . Cordials and Liqueurs ........................ . 10. Beverages: Malt Beverages and Brewing Materials Beer ......................................... . Malt ......................................... . Cereal Adjuncts .............................. . Hops ........................................ . Brewing Sugars and Sirups ................... . Wort ......................................... . Yeast ........................................ . Brewers' Grains 11. Beverages: Wines ............................... . Preservatives ................................. . Flavors ...................................... . 12. Beverages: Nonalcoholic and Concentrates ....... . 13. Cacao Bean and Its Products .............. " ..... . Shell ......................................... . Cacao Products Processed with Alkalies ....... . Chocolate Liquor ............................. . Fat .......................................... . Dairy Ingredient Constituents ................. . Saccharine Ingredients Other Than Lactose .... . Starch ....................................... . 143 147 147 159 162 162 171 177 178 180 181 182 183 185 192 193 194 199 200 205 205 205 206 207 208 Chocolate Products. . . . . . . . . . . . . . . . . . . . . . . . . . . . 209 Theobromine. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 209 14. Cereal Foods. . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . 211 Wheat Flour. . . . .. . . . . . . . . . . . . . . . . . . . . . .. . . . . . . 211 Wheat, Rye, Oats, Corn, Buckwheat, Rice, and Barley and Their Products Except Cereal Adjuncts .................................... 220 Soybean Flour ................................ 223 Bread....... . . . .... . ..... ..... ... . . . . . .... . ... 223 Baked Products. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 226 PAGE Baked Products Other Than Bread (Not Containing Fruit) ............................ 227 Fig Bars and Raisin-Filled Crackers ............. 227 Macaroni, Egg Noodles, and Similar Products. . . 228 15. Coffee and Tea ....................... " . . . . . .. . . . 233 Green Coffee. . . . . . . . . . . . . . .. . . . . . . . . . . . . . .. . . . 233 Roasted Coffee . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 233 Tea........................................... 235 16. Dairy Products. . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . 238 Sampling ..................................... 238 Milk.......................................... 240 Automated Methods . . . . . . . . . . . . . . . . . . . . . . . . . . . 246 Cryoscopic Methods . . . . . . . . . . . . . . . . . . . . . . . . . . . 249 Penicillins in Milk. . . . . . . . . . .. . . . . . . . . . . . . . . . . . . 255 Cream........................................ 256 Evaporated Milk. . . . . . . . . . . . . . . . . . . .. . . . . . .. . . . 258 Sweetened Condensed Milk ........ " . . . . . .. . . . 259 Dried Milk, Nonfat Dry Milk, and Malted Milk ... 259 Butter. .... ... .... . .. . . . . .... . ... . ....... . ..... 260 Cheese....................................... 264 Ice Cream and Frozen Desserts. . . . . . . . . . . . . . . . . 272 17. Eggs and Egg Products. . . . . . . .. . . . . . . . . . . . . . . . . . . 275 18. Fish and Other Marine Products ....... " . . . .. ..... 285 19. Flavors .......................................... 306 Alcohol ....................................... 306 Vanilla Extract and Its Substitutes .............. 306 Lemon, Orange, and Lime Extracts and Flavors. 313 Lemon and Orange Oils. . . . .... . ..... ... . ... . . . 316 Almond Extract. . .... . ... . . .. ... . ....... . ..... . 318 Cassia, Cinnamon, and Clove Extracts. ... . .... . 319 Ginger Extract. . ..... ..... . .... . . .... . . . . .... .. 319 Peppermint, Spearmint, and Wintergreen Extracts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 319 Anise and Nutmeg Extracts .................... 319 Other Extracts and Toilet Preparations. . . . . . . . . . 319 20. Food Additives: Direct. . . . . . . . . . . . . . . . . . . . . . . . . . . . 323 Acidulants .................................... 323 Antioxidants .................................. 323 Chemical Preservatives ........................ 325 Emulsifying Agents. . . . . . . . . . . . . . . .. . . . . . . .. . . . 343 Enzymes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 344 Miscellaneous. . . . . . . . . . . . . . . . . . . . .. . . . . . . .. . . . 345 Nonnutritive Sweeteners. . . . . . . . . . . . . . . . . . . . . . . 347 Nutrients. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 352 Solvents ...................................... 352 21. Food Additives: Indirect. . .. .... . .... .. . . . ... ..... 354 22. Fruits and Fruit Products ......................... 359 Moisture. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 361 Solids........................................ 362 Potassium .................................... 363 Sodium....................................... 364 Phosphorus . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 364 Betaine ....................................... 365 Fruit Acids .................................... 366 Sugars........................................ 369 Anthocyanins ................................. 370 vi
  8. 8. PAGE PAGE Lemon Juice .................................. 372 Carbaryl .................................... 483 Sulphenone . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 485 23. Gelatin, Dessert Preparations, and Mixes . . . . . . . . . . 374 Perthane . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 485 DDT........................................ 485 24. Meat and Meat Products ......................... 376 Dichlone ................. . . . . . . . . . . . . . . . . . . . 487 Meat.......................................... 376 Guthion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 488 Meat Extracts and Similar Products. . . . . . . . . . . . . 383 Dodine...................................... 488 Ethylenethiourea ............................ 488 25. Metals and Other Elements as Residues in Foods .. 385 Glyodin . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 489 Antimony ..................................... 385 Hexachlorobenzene and Mirex ............... 490 Arsenic ....................................... 385 Malathion. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 490 Cadmium ..................................... 388 Maleic Hydrazide .................. . . . . . . . . . . 490 Copper....................................... 391 Methoxychlor ............................... 491 Fluorine. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 392 Mirex . . . . . . . .. . .. . . ... . . . . . . .. . . . . ... . .. . . . . 492 Lead.......................................... 397 Monofluoroacetic Acid. . . . . . . . . . . . . . . . . . . . . . . 492 Manganese ................................... 405 Naphthaleneacetic Acid. . . . . . . . . . . . . .. . . . . . . . 493 Mercury ...................................... 405 Nicotine .................................... 494 Nickel. . .. . ... ... . .... . .. . . .. . ... . ... . . . .. . ... . 409 Parathion ................................... 495 Selenium ..................................... 409 Piperonyl Butoxide .......................... 495 Tin........................................... 410 Thiram...................................... 495 Titanium . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 411 Zinc.......................................... 411 30. Spices and Other Condiments .................... 497 Spices........................................ 497 26. Natural Poisons . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 414 Mycotoxins ................................... 414 Aflatoxins . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 415 Prepared Mustard ............................. 500 Dressings for Foods ........................... 501 Vinegars. . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . 503 Minicolumn Detection Methods .............. 417 Quantitative Methods. . . . . . . . . . . . . . . . . . . . .. . . 418 Aflatoxin M, . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 427 Ochratoxins . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 428 Patulin. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 430 Sterigmatocystin ............................ 431 Zearalenone . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 432 Marine Toxins. . . . . . . . . . . . . . . . . . . . . .. . . . . . . .. . . 433 Phytotoxins ................................... 433 31. Sugars and Sugar Products. . . . . . . . . . . . . . . . . . . . . . . 506 Sugars and Sirups. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 506 Molasses and Molasses Products. .. . . . .. . .. . .. . 516 Confectionery. ... .. . . . .. . . .. . .. . .. . . . .. . . . .. . . 519 Honey........................................ 520 Maple Products ............................... 528 Sugar Beets. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 532 Starch Conversion Products. . . . . . . . . . . . . . . . . . . . 532 27. Nuts and Nut Products ........................... 435 32. Vegetable Products, Processed. . . . .. . . . .. .. . . .. .. . 537 Canned Products .............................. 537 Peanut Butter ................................. 435 Shredded Coconut. . .. . . . . . . . . . . . . . . . . . . . . . . . . . 436 Dried Vegetables .............................. 542 Frozen Vegetables. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 543 28. Oils and Fats. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 437 33. Waters; and Salt . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 547 .. ?hysical Constants ............................ 437 Water......................................... 547 Chemical Constants ........................... 438 Salt........................................... 565 Acid Constituents. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 441 Sterols. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 452 34. Color Additives .................................. 568 Tests for Specific Oils. . . . . . . . . . . . . . . . . . . . . . . . . . 456 Separation and Identification of Color Additives Chick Edema Factor ........................... 459 in Foods, Druq!'; and Cosmetics. . . . . . . . . .. . . . 568 Mono- and Diglycerides . . . . . . . . . . . . . . . . . . . . . . . . 461 Analysis Of r brcial Synthetic Organic Color t:'laxseed ...................................... 464 Additives .....:.............................. 570 29. Pesticide Residues ............................... 466 35. Cosmetics ....................................... 582 Multiresidue Methods ......................... 466 General Methods. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 582 General Method for Organochlorine and Deodorants and Anti-Perspirants ............... 583 Organophosphorus Pesticides. . . . . . . . . . . . . . 466 Dipilatories . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 587 Multiple Residue Methods for Face Powders ................................. 587 Organophosphorus Pesticides. . . . . . . . . . . . . . 476 Hair Preparations. . . . . . . . . . . . . . . . . . . . . . .. . . . . . . 587 Multiple Residue Methods for Fumigants ..... 480 Suntan Preparations. . . . . . . . . . . . . . . . . . . . . . . . . . . 589 Multiple Residue Method for Aryl N- Vanishing Cream. . . . . . . . . . . . . . . . . . . . . . .. . . . . . . 589 Methylcarbamate Insecticides .............. 480 Bioassay. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 590 Methods for Individual Residues ............... 481 Benzene Hexachloride ....................... 481 36. Drugs: General. . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . 591 Biphenyl .................................... 481 General Directions. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 591 Aramite . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 483 Solvents ...................................... 591 Captan ...................................... 483 Halogenated Compounds. . . . . . . . . . . . . . . . . . . . . . 592 vii
  9. 9. PAGE Inorganic Drugs ............................... 594 Mydriatics and Myotics ........................ 604 Microscopic Tests ............................. 604 37. Drugs: Acidic .................... '" ........ '" .. 614 Acids......................................... 614 Antipyretic Drugs. .... . ... . ... ... . . ..... ..... .. 615 Hypnotic Drugs ................. " . .. . ... ..... . 619 Phenolic Drugs. . . . . .. . . . . . . . . . . . . . . . . . . . . . .. . . 625 Sulfonamide Drugs. .. . . . . . . . . . . . . . . . . . . . . . .. . . 629 Other Imide Drugs. . . . . . . . . . . . . . . . . .. . . . . . . .. . . 631 38. Drugs: Alkaloid and Related Bases ................ 636 Alkaloids, Opium. . . .. . . . . . . . . . . . . . . . . . . . . . . . . . 636 Alkaloids Other Than Opium ................... 639 Other Bases. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 649 39. Drugs: Neutral ................................... 667 Steroids and Related Hormones. . . . . . . . . . . . . . . . 667 Nonalkaloidal Vegetable Drugs and Their Derivatives. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 674 Miscellaneous. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 678 40. Drugs: Illicit. .. .. ... . . ..... ... .... . . .... . . . ... .. . . 685 41. Drugs and Feed Additives in Animal Tissues. . . . . . . 688 ANOT......................................... 688 Arsenic ....................................... 688 Clopidol ...................................... 689 Decoquinate .................................. 690 Ethoxyquin . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 691 Melengestrol Acetate .......................... 691 Nalidixic Acid ................................. 693 Zoalene . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 694 42. Drugs in Feeds . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 695 Qualitative Tests .............................. 695 Arsenic ....................................... 695 Cyzine ........................................ 696 Aklomide ..................................... 697 p-Aminobenzoic Acid. . . . . . .. . . . . . . . . . . . . . . . . . . 697 Enheptin ... . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 698 Amprolium ............................... " . . . 698 Arsanilic Acid ................................. 699 Bithionol . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 699 Buquinolate . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 699 Cadmium Anthranilate. . . . . . . . . . . . . . . . . . . . . . 700 Carbadox ..................................... 700 Decoquinate .................................. 700 Dibutyltin Dilaurate ., ..................... " . . . 701 Diethylstilbestrol .............................. 702 Nitrophenide ....... . Nitarsone .......... . Phenothiazine ...... . Piperazine .......... . Pyrantel Tartrate ... . Racephenicol ....... . Reserpine ....... " .. Ronnel .............. , Roxarsone .......... , Sulfonamide Drugs .. Thiabendazole ....... , Zoalene ............. , Antibiotics .......... , 43. Vitamins and Other Nutri Chemical Methods ... Microbiological Metho Bioassay Methods ... Nutritionally Related C 44. Extraneous Materials: IsCl General ............ . Beverages and Bevera Dairy Products ..... . Nuts and Nut Product~ Grains and Their Prodl Baked Goods ....... . Breakfast Cereals ... . Eggs and Egg Product Poultry, Meat, and Fisl Products ......... . Fruits and Fruit Produ( Sugars and Sugar Prol Vegetables and Vegetc Spices and Other ConI Animal Excretions .. . Miscellaneous ...... . 45. Forensic Sciences ..... . Latent Fingerprints .. Glass Fragments .... Mineral Wool Insulatio Voice Print Identificati( 46. Microbiological Methods Eggs and Egg Product Frozen, Chilled, Precoe Commercial Sterility 0 Thermophilic Bacterial Clostridium perfringen Salmonella . ........ . Optical Somatic Cell C
  10. 10. FIGURE 1:01. 2:01. 2:02. 2:03. 2:04. 2:05. 2:06. 2:07. 2:08. 3:01. 3:02. 3:03. 3:04. 3:05. 3:06. 3:07. 4:01. 4:02. 6:01. 6:02. 6:03. 6:04. 6:05. 6:06. 6:07. 6:08. 6:09. 7:01. 7:02. 7:03. Illustrations Apparatus for Automatic Filtration and Measurement of Lime Solutions ........................................... . Sampling Pattern ................................................ " ............................................. . Sampling Cup ..... " ................................... , ........ " ............................................. . Missouri and Indiana Weighted Restricted-fill Fluid Fertilizer Sampling Bottles Designed to Fill While Being Lowered (and Raised) in Storage Tanks ................................................................................... . Sampling Apparatus for Ammoniacal Solutions, Including "Quick Coupler" for Attaching to Storage Tanks .......... . Apparatus for Control of Water Pressure ......................................................................... . Flow Diagram for Automated Analysis for Phosphorus ........................................................... . Flow Schematic for K20 in Fertilizers ............................................................................ . Apparatus for Elution of Resin Column .......................................................................... . Suction Device Used in Micro Method for Determining Calcium ................................................... . Schematic Drawing of Air Flow System Used in Semiautomated Analysis for Fluoride ............................. . Flow Diagram for Semiautomated Analysis for Fluoride .......................................................... . Schematic Drawing of Microdistillation Apparatus ................................................ , ............... . Microdistillation Column ........................................................................................ . Apparatus for Determining Lignin ............................................................................... . Distillation Apparatus ........................................................................................... . Transfer Loop and Manner of Using in Phenol Coefficient Technic ................................................ . Stainless Steel Spindle for Winding Test Fabric .................................................................. . Delivery Assembly for Sampling Pressurized Containers .......................................................... . Apparatus for Distilling Arsenious Chloride ...................................................................... . Apparatus for Determining Fluorine ............................................................................. . Partition Column and Solvent Evaporator ........................................................................ . Melting Point Apparatus ........................................................................................ . Distillation Apparatus ........................................................................................... . Carbon Disulfide Evolution Apparatus .................................................................... ..... . Absorption System for Thiram ............................................................................. : .... . Filtration Apparatus ............................................................................................ . Flow Diagram for Semiautomated Analysis for Crude Protein ..................................................... . Agitator ........................................................................................................ . Oklahoma State Filter Screen ................................................................................... . PAGE 2 7 7 7 8 9 12 20 26 32 41 42 43 43 48 54 57 67 72 73 76 94 94 99 110 111 122 128 131 133 7:04. Modified California State Buchner Funnel... .... . ... . ... . .. . . . ... .... . .... . ... .... . . . .... ... . . ... ... .. . .... ... ... . 133 7:05. Continuous Heater for Distilled Water, 1.25% Alkali, and 1.25% Acid ............................................... 133 8:01. Chittick Apparatus for Gasometric Determination of Carbon Dioxide ............................... :-................ 143 9:01. 100 mL and 50 mL Pycnometers ................................................................................. 148 9:02. Williams Tube. . . . . . . . . . . .. . . . . . . .. . . . . . . . . . . . . . .. . . . . . . .. . . . . . . . . . . . . . .. . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 149 9:03. Steam Distillation Flask. . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 156 9:04. Apparatus for Determining Hydrogen Cyanide in Distilled Spirits................................................... 158 10:01. Absorption Buret................................................................................................ 166 11 :01. Distillation Apparatus for Chemical Determination of Alcohol in Wine .............................................. 186 11 :02. Volatile Acid Still (Cash Still) .......................... " ............ '" ..................................... '" . . 188 11 :03. Carbon Dioxide Apparatus; Manometric Method ...................................... '" ............... '" . ...... 190 11 :04. Carbon Dioxide Apparatus; Volumetric Method ........ '" ................ '" . '" . . . . ...... . . ...... ... .... ... . .. . . 192 12:01. Continuous Extraction Apparatus .......... " . '" ............................ ,. . . ..... ... . . ... . .. . ... ... . . ... ... .. 195 13:01. Spiral Vessel Sections. . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . .. . . . . . . . .. . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 203 13:02. Stone Cells ..................................................................................................... 204 13:03. Graph Used in Correcting Cuprous Oxide for Effect of Sucrose ........................................ '" . . .. . ... .. 207 16:01. Apparatus for Drying Pentabromacetone by Aspiration ............................................................ 241 16:02. Liquid Extractor ...................................... '" . " ....................................... , ... . . .. .... .. 242 16:03. Flow Diagram for Determination of Fat in Milk ......... '" ......... , ..... '" . .... . . .... ... . .... ... ... . .. . . ... . .. . . 247 16:04. Modified Jones Reductor ........................................................................................ 266 16:05. Modified Plastic Desiccator ...................................................................................... 273 18:01. Extraction Apparatus............................................................................................ 291 18:02. Steam Distillation Assembly ..................................................................................... 292 ix
  11. 11. FIGURE PAGE 18:03. Muscle Bath .................................................................................................... 294 18:04. Electrophoresis Cabinet. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . 300 18:05. Disc Electrophoresis Apparatus .................................................................................. 300 18:06. Key to Identification of Canned Salmon Species by Scale Characteristics ........................................... 302 18:07. Sockeye (Red) Salmon Scale (Oncorhynchus nerka) ............................................................... 303 18:08. Chinook (King) Salmon Scale (Oncorhynchus tshawytscha) ........................................................ 304 18:09. Coho (Silver) Salmon Scale (Oncorhynchus kisutch) . . . . .. . . . . . .. .. . . . ... . . .. . . ... . . . . ... . . .. . .. ... . .. . . . .. . . ... . . . 304 18:10. Chum Salmon Scale (Oncorhynchus ketal ........................................................................ 304 18:11. Pink Salmon Scale (Oncorhynchus gorbuscha) ........ ............................... .... ................... ...... 304 19:01. Wilson Flask.................................................................................................... 315 19:02. Oil Separator Trap. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . .. . . . . . .. . . . . . . . . . . . . . . . . . . . . . .. . . . . 320 20:01. Steam Distillation Apparatus. . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 326 20:02. Placement of Slides on Template for Applying Silica Gel Coating .................................................. 327 20:03. Steam Distillation Apparatus. . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . 338 20:04. Apparatus for Modified Monier-Williams Method for Sulfur Dioxide. . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . 339 20:05. Alternative S02 Absorber. . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . .. . . . . . . .. . . . . . .. . . . . 339 20:06. Gas Chromatograms of TBS, DBS, and TBS + DBS . . . . . .. . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 346 20:07. Microsampling Die .............................................................................................. 348 20:08. GLC Effluent Collection Trap for Determination of Cyclohexylamine ................................................ 350 21 :01. Test Cell. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . .. . . . . . . . . . . . 356 21:02. Oven Rack...................................................................................................... 357 22:01. Apparatus for Determining Volume of Frozen Fruits by Displacement............................................... 359 22:02. Capillary Viscometer ............................................................................................ 361 22:03. Electrical Circuit Diagram for Dried Fruit Moisture Tester.. . . . . ... . . .. . . ... . . .... . . .... .. .. . . ... . ... . ... . . . .. . . ... . 361 22:04. Connecting Tube Adapter for Direct Distillation ................................................................... 370 23:01. 0.5 Inch Bloom Gelometer Plunger ............................................................................... 374 23:02. 1.0 Inch Bloom Gelometer Plunger. . . . . .. .. . ... .. .. . . ... ... . . . ... . ... . . . .. . . . .. . . . . . ... ... . . . ... . .. . ... . . . .... ... 375 24:01. Helix Inlet Manifold. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . 377 24:02. Phosphorus Analytical Manifold. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . 378 24:03. Nitrogen Analytical Manifold. . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . .. . . . . . . .. . . . . . . . . . . . . . . . . . . . . . .. . . . 379 25:01. Arsenic Apparatus. . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . .. . . . . . . . . . . . . . .. . . . . . . .. . . . . . . . . . . . . . .. . . . . . . . . . . . 386 25:02. Apparatus for Flameless Atomic Absorption Analysis. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 406 25:03. Digestion Vessel ................................................................................................ 407 25:04. Special Digestion Apparatus for Mercury Residues. . . . . . . . . . . . . .. . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . 408 26:01. Spotting and Scoring Patterns for 2-Dimensional TLC Plates. . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . 424 26:02. Plate Scraper for Removing Adsorbent From TLC Plates .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 424 26:03. Schematic Showing Parts of Egg and Modes of Test Material Introduction. . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . .. . . . 426 28:01. Titer Stirring Assembly. .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . .. . . . 439 28:02. Liquid-Liquid Extractor. . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . .. . . . 442 28:03. Apparatus for Determining Reichert-Meissl and Polenske Values ................................................... 443 28:04. Constant Temperature Bath and Accessories. . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . .. . . . 444 28:05. Distribution Heads; Manifold. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 445 28:06. Glass Micro Filter for Sterol Acetate Precipitates .................................................................. 452 28:07. Crystalline Forms of Free Sterols. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . 453 28:08. Apparatus for Determining Melting Point ......................................................................... 458 29:01. KCI Thermionic Detector Coil for In-series Dual Detection System .................................................. 468 29:02. KCI Thermionic Detector Coil for Parallel and In-series Split Dual Detection Systems ................................ 469 29:03. In-series Split Dual Detection System. . . . . . . . . . . .. . . . . . . .. . . . . . . . . . . . . . . . . . . . . . .. . . . . . .. . . . . . . .. . . . . . . . . . . . . . . . . . . 469 29:04. Parallel Dual Detection System. . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . 469 29:05. In-series Dual Detection System. .. . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . .. . . . . . . . . . . . . . . . . . . 469 29:06. Sweep Co-distillation Apparatus. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 477 29:07. Evaporative Concentrator. . . . . . . .. . . . . . . . . . . . . . .. . . . . . . .. . . . . . . . . . . . .. . . . . . . . . .. . . . . . . . . . . . . . .. . . . . . . .. . . . . . . . . . . 484 29:08. Distillation Apparatus for Maleic Hydrazide Determination ......................................................... 491 30:01. Apparatus for Volatile Oil in Spices. . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . .. . . . . . . .. . . . . . . . . . . 498 31 :01. Fractionator..................................................................................................... 506 31 :02. Carbon Combustion and Purification System. . . . . . . . . . . . .. . . . . . . .. . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . 527 31 :03. Distillation Apparatus for Determining Formaldehyde in Maple Sirup.. . . .... . ... .. . . . ... . ... . . ... . .. . . ... . ... . ... . . 530 33:01. Apparatus for Determination of Mercury by Flameless Atomic Absorption. . . . . . . .. . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . 560 33:02. Phosphorus Manifold. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 563 34:01. Titanous Chloride Titration Apparatus ............................................................................ 574 34:02. Sulfiding Apparatus ............................................................................................. 579 36:01. Apparatus for Determining Arsenic in Iron-Arsenic Tablets. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . 594 36:02. Flow Diagrams for Semiautomated Analysis for Ferrous Sulfate. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . .. . . . . . . . . . . 601 37:01. Bromine Apparatus.............................................................................................. 619 x
  12. 12. FIGURE PAGE 37:02. Flow Diagram for Automated Analysis for Acenocoumarol, Dicumarol, Phenprocoumon, Potassium Warfarin, and Sodium Warfarin . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 629 38:01. Flow Diagram for Semiautomated Fluorometric Analysis for Reserpine............................................. 646 38:02. Flow Diagram for Phenylephrine Hydrochloride ................................................................... 661 38:03. Assembly of Debubbler . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 662 39:01. Flow Diagram for Semiautomated Analysis for Prednisolone or Prednisone. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 674 39:02. Flow Diagram for Automated Analysis for Digoxin ................................................................ 675 39:03. Scrubber Trap for Ammonia Distillation .......................................................................... 679 39:04. Flow Diagram for Automated Analysis of Methenamine and Methenamine Mandelate. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 683 43:01. Flow Diagram for Automated Analysis for Niacin and Niacinamide.. .... . .... ..... . . . ........ . .... .... ... . . ... . ... . 745 43:02. RRR-a-Tocopherol . . . . . . . .. . . . . . . .. . . . . . .. . . . . . . .. . . . . .. . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . .. . . . . . . .. . . 752 43:03. Line Test Chart. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 771 43:04. Radii Sections Scored According to Line Test Chart ............................................................... 772 44:01. Mechanical Butter Stirrer ........................................................................................ 781 44:02. Wildman Trap Flask .......................................................................... , .... ........ . ... .. 781 44:03. Rot Fragment Counting Slide .................................................................................... 782 44:04. Sediment Filtering Apparatus, Unassembled ...................................................................... 786 44:05. Sediment Filtering Apparatus, Assembled ........................................................................ 786 44:06. Rot Fragments from Tomato Puree ...................... , . . . . . . .. . . . . . . . . . . . . . .. . . . . . . .. . . . . . . . . . . . . . .. . . . . . . .. . . 800 44:07. Rot Fragments from Tomato Puree. . . . . . .. . . . . . . .. . . . . ... . . . . . . .. . . . . . . . . . . . . . .. . . . . . . .. . . . . . . . . . . . . . .. . . . . . . . . . . 801 44:08. Mold Filaments in Tomato Products. . . . . .. . . . . . . .. . . . . . .. . . . . . . .. . . . . . . . . . . . . . .. . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . 802 44:09. Insect Penetration of Packaging .................................................................................. 817 46:01. Plastic Template Schematic for Microslide Assembly.............................................................. 842 46:02. Arrangement of Antisera and Homologous Reference Enterotoxins . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 843 46:03. Examples of 4 Possible Reactions in Bivalent Detection System .................................................... 844 46:04. Effect of Amount of Enterotoxin in Test Preparation on Development of Reference Line of Precipitation .............. 845 46:05. Appearance of Microslide Gel Diffusion Test as Monovalent System ............................................... 845 46:06. Precipitate Patterns in Microslide Gel Diffusion Test Demonstrating Nonspecific (Atypical) Lines of Precipitation. . . . . . 845 46:07. Optical Somatic Cell Counter Flow Diagram ....................................................... , . . . .. . . . . . . . . . . 846 46:08. Optical Somatic Cell Counter Flow Diagram. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 848 46:09. Optical Somatic Cell Counter Flow Diagram. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 849 47:01. Combustion Tube............................................................................................... 853 47:02. Carbon and Hydrogen Apparatus.... . . . .......... ... ......... ........... .... ..... . . . ... . .... .... ....... ....... . .. 855 47:03. Upper Section of Distilling Apparatus. . . . .. . . . . . . . . . . . . ... . . . . . . .. . . . . . .. . . . . . . .. . . . . . . . . . . . . . .. . . . . . . .. . . . . . . . . . . 857 47:04. Gravimetric Setup for Oxygen Determination ..................................................................... 859 47:05. Quartz Reaction Tube and Filling for Oxygen Determination ....................................................... 859 47:06. Details of Modified Clark Apparatus .............................................................................. 862 47:07. Modified Clark Apparatus. . . . . . . .. . . . . . . .. . . . . . . . . . . . . ... . . . . . . .. . . . . . .. . . . . . . .. . . . . . . . . . . . . . .. . . . . . . .. . . . . . . . . . . 863 48:01. Cross-section of Marinelli Beaker. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 869 xi
  13. 13. Collaborative Study Procedures of the Association of Official Analytical Chemists The Association of Official Analytical Chemists (AOAC) is a unique, nonprofit scientific organization whose primary purpose is to serve the needs of government regulatory and research agencies for analytical methods. The goal of the Association is to provide methods which will perform with the necessary accuracy and precision under usual laboratory conditions (1). Since its formation in 1884 the AOAC has provided a mechanism to select methods of analysis from published literature or develop new methods, collaboratively test them through inter- laboratory studies, approve them, and publish the approved methods for a wide variety of materials relating to foods, drugs, cosmetics, agriculture, forensic science, and products affecting the public health and welfare. Its membership is composed of scientists from Federal, State, Provincial, and other regulatory bodies who work within the AOAC's established procedures as researchers, methods collaborators, and committee members. Although most of the members are from North America, many nations throughout the world are represented. The AOAC has almost a century of experience in utilizing the collaborative study as a means of determining the reliability of analytical methods for general purposes and, especially, for regulatory purposes. In fact, the AOAC's major contribution to analytical science has been to bring the collaborative study technique for the validation of analytical methods to a high degree of perfection. In such a study, laboratories analyze identical sample sets which cover the range of applicability of a method previously selected as being useful and practical. The purpose of the study is to establish the characteristics of the methods with respect to accuracy, precision, sensitivity, range, specificity, limit of detection, limit of reliable measurement, selectivity, practicality, and similar attributes, as required. ORGANIZATION AND PROCEDURES FOR AOAC COLLABORATIVE STUDIES The collaborative study is organized and directed by an analyst designated as the Associate Referee for the specific subject under investigation. Currently, some 600 Associate Referees appointed by the Association are responsible for as many topics. An Associate Referee is selected for his knowledge, interest, and experience in the subject matter field. He operates under the scientific guidance, support, and administrative supervision of a General Referee, who is in turn responsible for a product area. The Associate Referee reviews the literature and selects one or two of the better analytical methods available, modifying them as needed. Alternatively, he may develop or adapt a method used in his laboratory for the analyte and matrix under study, testing it thoroughly in his laboratory before designing a collaborative study. The General Referee is kept informed of such preliminary studies. The samples analyzed in a collaborative study are normally prepared and distributed to the participants by the Associate Referee. The Association follows the recommendations of You- den (2) that not fewer than five laboratories participate and that a minimum of six sample materials be sent to each. These are xii minima and, in practice, both are usually exceeded. In addition, a reference or practice sample is included, where possible. Laboratories with at least some experience in the general subject matter are selected as collaborators. Because the objec- tive of the study is to standardize the method, as contrasted to standardizing the analyst (3). all analysts are instructed to follow the method exactly as written even though they may not concur with the Associate Referee's selection among possible alterna- tives. The level ofthe analyte in the samples is usually unknown to the participants. All individual results obtained by the collaborators are re- ported to the Associate Referee, who compiles and evaluates them. Since statistical treatment of the data is considered essential in a rigorous evaluation of the method for accuracy, precision, sensitivity, and specificity, it is now required for all studies. The Association considers this of such importance that it provides statistical assistance in all cases where it is otherwise unavailable to the Associate Referee. A statistical manual (4) is also provided. The Associate Referee makes the initial judgment on the performance of the method. If he recommends approval, it passes to the General Referee and then to a committee of experts. If both recommend approval, the method is presented at the Association's annual business meeting for vote by the membership. Approved methods and supporting data are published in the Journal of the Association of Official Analytical Chemists. They are subject to scrutiny and general testing by other analysts for at least a year before final adoption. They may be modified and restudied collaboratively as needed, should feedback from gen- eral use reveal flaws in the method or in its written set of directions. Approved methods are included in the Association's "Official Methods of Analysis", a book of some 1000 pages which is updated every 4-5 years. The preceding summary of AOAC's modus operandi recog- nizes the need for healthy skepticism toward results obtained by analytical methods which have not undergone such rigorous scrutiny and interlaboratory testing of their accuracy, precision, dependability, specificity, and practicality. SELECTION OF METHODS FOR STUDY A certain degree of variability is associated with all measure- ments. Much of the research on analytical chemistry is an attempt to minimize that variability. But there are many different types of variability in analytical work. We often find that when we attempt to minimize one kind, we must necessarily permit expansion in another kind. In practical analytical chemistry, the problem often comes down to which variability is to be mini- mized. Some examples ofthis point may be helpful. In atomic weight determination, everything-especially practicality-is sacrificed for accuracy. A high degree of accuracy and practicality is required in the assay of precious metals, but the fire assay used is generally applicable to little else besides metals and minerals.
  14. 14. In clinical chemistry, within-laboratory precision (repeatability) is critical, and often is of greater interest to clinical laboratories than absolute accuracy or agreement with the values of other laboratories (reproducibility). In drug analysis, a high degree of accuracy is required in the therapeutic range because the analytical values determining the identity, strength, quality, and purity of pharmaceutical preparations, as laid down in phar- macopoeial specifications, are directly related to clinical value. With polynuclear hydrocarbons, specificity is important, since some of these compounds are carcinogenic while others are not. In applying the famous Delaney clause of the United States Federal Food, Drug, and Cosmetic Act, all attributes of the analytical methods are secondary to the detection of extremely small concentrations (detectability), or to exhibiting a high degree of response for small changes in concentration (sensi- tivity). There is a very special case involving accuracy, where the "true value" is determined by the method of analysis. Many legal specifications and standards for food and agricultural products define ill-defined components such as moisture, fat, protein, and crude fiber in terms of reference methods. There- fore, the precision of these methods becomes the limiting factor for their performance. In fact, most analyses involved in com- mercial transactions require primarily that the buyer and seller agree on the same value (analytically and economically), re- gardless of where it stands on an absolute scale. The point of these examples is that although methods of analysis are characterized by a number of attributes-accuracy, precision, specificity, sensitivity, detectability, dependability, and practicality-no method is so flawless that all these qualities can be maximized simultaneously. For any particular analysis, the analyst must determine, on the basis of the purpose of the analysis, which attributes are essential and which may be compromised. Unfortunately, the literature is replete with examples indicat- ing that an individual analyst, and especially the originator of a method of analysis, is not an unbiased judge of the relative merits of the methods of analysis which he develops and uses. In our experience, the collaborative study provides impartial data on the suitability of the method. The data, in many cases, speak for themselves. The collaborative study, or ring test or round robin test, as it is called in other organizations, provides the basic information on the performance of analytical methods. The extent of the information will depend on the number of samples provided, the number of analyses performed, and the number of labora- tories participating. The data should be unbiased because the composition of the samples is known only to the administrator of the study. Some of the requirements of the study and their relationship to the characteristics and attributes of the method are as follows: (1) Accuracy. Samples must be of defined composition (by spiking, by formulation, or by analytical consensus). (2) Specificity. Samples should contain related analytes. (3) Sensitivity. Samples should differ from each other or from negative samples by a known amount. (4) Applicability. Samples should include the concentration range and matrix components of interest. (5) Blanks. Samples should include different matrices with "none" of the component of interest. (6) Precision. Instructions should request replicate analyses by the same or different analysts in the same laboratory, preferably on different days. By far a better procedure is to include "blind" (unknown to the analyst) replicate samples in the series. (7) Practicality. Instructions should request information as to xiii the actual and elapsed time required for the analyses; the availability of reagents, equipment, and standards; and any necessary substitutions. When practice samples are included, the number of analyses required to achieve the stated recovery and repeatability, should be reported. PROCEDURAL DETAILS OF COLLABORATIVE STUDY As numerous beginners in this field have discovered, much preliminary work must be done before sending out samples: (1) The method must be chosen and demonstrated to apply to the matrices and concentrations of interest. (2) The critical variables in the method should have been determined and the need for their control emphasized [a rug- gedness test (5) is useful for this purpose]. (3) The method should be written in detail by the Associate Referee and tested by an analyst not previously connected with its development. (4) Unusual standards, reagents, and equipment must be available from usual commercial sources of supply, or sufficient quantities must be prepared or obtained to furnish to the participants. (5) The samples must be identical and homogeneous so that the analytical sample error is only a negligible fraction of the expected analytical error. (6) A sufficient number of samples must be prepared to cover typical matrices and the concentration range of interest (toler- ance, maximum or minimum specifications, likely levels of occurrence, etc.). (7) Samples must be stable and capable of surviving the rigors of commercial transportation. (8) Reserve samples should be prepared and preserved to replace lost samples and to permit reanalysis of samples con- sidered as outliers to attempt to discover the cause of abnormal results. (9) The instructions must be clear. They should be reviewed by someone not connected with the study to uncover potential misunderstandings and ambiguities. (10) If the analyte is subject to change (e.g., bacterial levels, nitroglycerin tablets), provision must be made for all participants to begin the analysis at the same time. (11) Practice samples of a known and declared composition should be furnished with instructions not to analyze the un- knowns until a specified degree of recovery and repeatability (or other attribute) has been achieved. (12) Provision should be made when necessary for submis- sion of standard curves, tracings of recorder charts, or photo- graphs of thin-layer plates in order to assist in determining possible causes of error. OTHER TYPES OF INTERLABORATORY STUDIES This type of collaborative study, which is designed to deter- mine the characteristics of a method, must be carefully distin- guished from other types of interlaboratory studies which by design or through ignorance provide other kinds of information. The most important types of other studies are: (1) Those studies which require the collaborators to investi- gate the variability of parts of methods or applicability to different types of samples. (An interlaboratory study is usually an inefficient way of obtaining this type of information.) (2) Those studies which permit an analyst to use any method he desires. Such studies invariably produce such a wide scatter of results that the data are of little value for evaluation of methods. They may be useful in selecting a method from a number of apparently equivalent methods, provided the purpose
  15. 15. is emphasized beforehand and the participants provide a de- scription of the method used in order to permit a correlation of the details of the methods with apparent biases and variabilities. (3) Those studies which are used for quality control purposes, whose participants are not permitted sufficient time to gain familiarity with the method, or who permit deviations to enter into the performance of the analyses on the grounds that the deviation is obviously an improvement which could not possibly affect the results of the analysis, or who claim to have a superior method. With this background information, it is now appropriate to introduce the following definitions which were agreed upon as part of the guidelines for collaboration between the AOAC and the Collaborative International Pesticide Analytical Council L~d. (CIPAC) (6). Collaborative study. An analytical study involving a number of laboratories analyzing the same sample(s) by the same method(s) for the purpose of validating the performance of the method(s). Preliminary interlaboratory study. An analytical study in which two or more laboratories evaluate a method to determine if it is ready for a collaborative study. Laboratory performance check. The analysis of very carefully prepared and homogeneous samples, normally of known active ingredient content, to establish or verify the performance of a laboratory or analyst. SUMMARY The collaborative study i's an experiment designed to evaluate the performance of a method of analysis through the analysis of a number of identical samples by a number of different laboratories. With proper design, it provides an unbiased eval- uation of the performance of a method in the hands of those analysts who will use it. A collaborative study must be distin- guished from those studies designed to choose a method or to determine laboratory or analyst performance. REFERENCES (1) AOAC, "Handbook of the AOAC", 4th ed., AOAC, Box 540, Benjamin Franklin Station, Washington, D.C. 20044, 1977. (2) W. J. Youden, "Accuracy of Analytical Procedures", J. Assoc. Off. Anal. Chern., 45, 169-73 (1962). (3) Harold Egan, "Methods of Analysis; An Analysis of Meth- ods", ibid., 60,260-7 (1977). (4) W. J. Youden and E. H. Steiner, "Statistical Manual of the AOAC: Statistical Techniques for Collaborative Tests. Plan- ning and Analysis of Results of Collaborative Tests", AOAC, Box 540, Benjamin Franklin Station, Washington, D.C. 20044, 1975. (5) W. J. Youden, "The Collaborative Test", J. Assoc. Off. Anal. Chern., 46, 55-62 (1963). (6) "Guidelines for Collaboration Between the Association of Official Analytical Chemists (AOAC) and the Collaborative International Pesticide Analytical Council Ltd. (CIPAC)", ibid., 57,447-9 (1974). BIBLIOGRAPHY Daniel Banes, "The Collaborative Study as a Scientific Concept", J. Assoc. Off. Anal. Chern., 52,203-06 (1969). William Horwitz, "Problems of Sampling and Analytical Meth- ods", ibid., 59, 1197-203 (1976). Reprinted with permission from: Analytical Chemistry (March 1978) 50, 337A-340A. Published 1978 American Chemical Society xiv
  16. 16. Definitions of Terms and Explanatory Notes Reagents (1) Term "H20" means distilled water, except where otherwise specified, and except where the water does not mix with the detn, as in "H20 bath." (2) Term "alcohol" means 95% ethanol by vol. Alcohol of strength x% may be prepd by dilg x mL 95% alcohol to 95 mL with H20. Absolute alcohol is 99.5% by vol. Formulae of specially denatured alcohols (SDA) used as reagents are as follows: SDA No. 100 parts alcohol plus 1 5 wood alcohol 2-B 3-A 12-A 13-A 23-A 30 0.5 5 5 10 10 10 benzene or rubber hydrocarbon solv. MeOH benzene ether acetone MeOH "Reagent" alcohol is 95 parts SDA 3-A plus 5 parts isopropanol. (3) Term "ether" means ethyl ether, peroxide-free by follow- ing test: To 420 mL ether in separator add 9.0 mL 1% NH4V03 in H2S04 (1+16). Shake 3 min and let sep. Drain lower layer into 25 mL g-s graduate, dil. to 10 mL with H2S04 (1 +16), and mix. Any orange color should not exceed that produced by 0.30 mg H20 2(1 mL of soln prepd by dilg 1 mL 30% H20 2to 100 mL with H20) and 9.0 mL 1% NH4V03in H2S04 (1 + 16). Peroxides may be eliminated by passing .;;700 mL ether thru 10 cm column of Woelm basic alumina in 22 mm id tube. (4) Reagents listed below, unless otherwise specified, have approx. strength stated and conform in purity with Recom- mended Specifications for Analytical Reagent Chemicals of American Chemical Society: Assay Sulfuric Acid . . . . . . . . . . . . . . . . . . . . . . . .. 95.0-98.0% H2S04 Hydrochloric acid .................... 36.5-38.0% HCI Nitric acid ........................... 69.0-71.0% HN03 Fuming nitric acid. . . . . . . . . . . .. . . . . . .. ;,,90% HN03 Acetic acid . . . . . . . . . . . . . . . . . . . . . . . . . .. ;,,99.7% HC2H30 2 Hydrobromic acid ......... " ..... . ... 47.0-49.0% HBr Ammonium hydroxide. . . . . . . . . . . . . . .. 28-30% NH3 Phosphoric acid. . . . . . . . . . . . . . . . . . . . .. ;,,85% H3P04 Where no indication of diln is given, reagent is of concn given above. (5) All other reagents and test solns, unless otherwise de- scribed in text, conform to requirements of American Chemical Society. Where such specifications have not been prepd, use highest grade reagent. When anhyd. salt is intended, it is so stated; otherwise the crystd product is meant. (6) Unless otherwise specified, phenolphthalein (phthln) used as indicator is 1% alc. soln; Me orange is 0.1 % aq. soln; Me red is 0.1 % alc. soln. (7) Directions for stdzg reagents are given in Chapter 50. (8) Unusual reagents not mentioned in reagent sections or cross referenced, other than common reagents normally found in laboratory, are italicized first time they occur in method. (9) Com. prepd reagentsolns must be checked for applicability to specific method. They may contain undeclared buffers, pre- servatives, chelating agents, etc. xv (10) In expressions (1 +2), (5+4), etc., used in connection with name of reagent, first numeral indicates vol. reagent used, and second numeral indicates vol. H20. For example, HCI (1 +2) means reagent prepd by mixing 1 vol. HCI with 2 vols H20. When one of reagents is solid, expression means parts by wt, first numeral representing solid reagent and second numeral H20. Solns for which the solv. is not specified are aq. solns. (11) In making up solns of definite percentage, it is understood thatx g substance is dissolved in H20 and dild to 100 mL. Altho not theoretically correct, this convention will not result in any appreciable error in any of methods given in this book. (12) Chromic acid cleaning soln is prepd by (1) adding 1 L H2SO. to ca 35 mL satd aq. Na2Cr207 soln; or (2) adding 2220 mL (9 Ib) H2S04 to ca 25 mL satd aq. Cr03 soln (170 g/100 mL). Reagents may be tech. grade. Use only after first cleaning by other means (e.g., detergent) and draining. Mixt. is expensive and hazardous. Use repeatedly until it is dild Of has a greenish tinge. Discard carefully with copious amts of H20. (13) All calcns are based on table of international atomic weights, 52.001. Apparatus (14) Burets, vol. flasks, and pipets conform to following Federal specifications (available from General Services Admin., Specification Activity 3F1, Washington Navy Yard, Bldg. 197, Washington, DC 20407): Buret NNN-B-00789a May 19, 1965 Flask, vol. NNN-F-00289d Feb 7, 1977 Pipet, vol. NNN-P-395c March 13, 1970 Pipet, measuring NNN-P-350c July 16,1973 See also NBS Circular 602, "Testing of Glass Volumetric Ap- paratus" (available as Com 73-10504 from NTIS, Springfield, VA 22151). (15) Standard taper ($) glass joints may be used instead of stoppers where the latter are specified or implied for connecting glass app. (16) Sieve designations, unless otherwise specified, are those described in Federal Specification RR-S-366e, Nov 9,1973 (avail- able from General Services Admin.). Designation" '100-mesh' (or other number) powder (material, etc.)" means material ground to pass thru std sieve No. 100 (or other number). Corresponding international std and US std sieves are given in Table 1. (17) Term "paper" means filter paper, unless otherwise spec- ified. (18) Term "high-speed blender" designates mixer with 4 canted, sharp-edge, stainless steel blades rotating at the bottom of 4-lobe jar at 10,000-12,000 rpm, or with equiv. shearing action. Suspended solids are reduced to fine pulp by action of blades and by lobular container, which swirls suspended solids into blades. Waring Blendor, or equiv., meets these require- ments. (19) "Flat-end rod" is glass rod with one end flattened by heating to softening in flame and pressing vertically on flat surface to form circular disk with flat bottom at end. (20) Designation and pore diam. range of fritted glassware are: extra coarse, 170-220 /-Lm; coarse, 40-60; medium, 10-15; fine, 4-5.5; Jena designations and pore diam. are: 1, 110 /-Lm; 2, 45; 3, 25; 4, 8.
  17. 17. (21) Unless otherwise indicated, temps are expressed as degrees Centigrade. Table 1. Nominal Dimensions of Standard Test Sieves (U.S.A. Standard Series) Sieve Designation Nominal Nominal International Sieve Wire Standard' U.S.A. Opening, Diameter, (ISO) Standard inches mm 12.5 mmb '/2 in.b 0.500 2.67 11.2 mm 7/'6 in. 0.438 2.45 9.5 mm 3/8 in. 0.375 2.27 8.0 mm 5/,6 in. 0.312 2.07 6.7 mm 0.265 in. 0.265 1.87 6.3 mmb '/. in." 0.250 1.82 5.6 mm No. 3'/2 0.223 1.68 4.75 mm No.4 0.187 1.54 4.00 mm No.5 0.157 1.37 3.35 mm No.6 0.132 1.23 2.80 mm No.7 0.111 1.10 2.38 mm No.8 0.0937 1.00 2.00 mm No. 10 0.0787 0.900 1.70 mm No. 12 0.0661 0.810 1.40 mm No. 14 0.0555 0.725 1.18 mm No. 16 0.0469 0.650 1.00 mm No. 18 0.0394 0.580 850 "me No. 20 0.0331 0.510 710 "m No. 25 0.0278 0.450 600 "m No. 30 0.0234 0.390 500 "m No. 35 0.0197 0.340 425 "m No. 40 0.0165 0.290 355 "m No. 45 0.0139 0.247 300 "m No. 50 0.Q117 0.215 250 "m No. 60 0.0098 0.180 212 "m No. 70 0.0083 0.152 180 "m No. 80 0.0070 0.131 150 "m No. 100 0.0059 0.110 125 "m No. 120 0.0049 0.091 106 "m No. 140 0.0041 0.076 90 "m No. 170 0.0035 0.064 75 "m No. 200 0.0029 0.053 63 "m No. 230 0.0025 0.044 53 "m No. 270 0.0021 0.037 a These standard designations correspond to the values for test sieve apertures recommended by the International Organization for Standard- ization, Geneva, Switzerland. b These sieves are not in the standard series but they have been included because they are in common usage. c 1000 I-'m = 1 mm. Standard Operations (22) Operations specified as "wash (rinse, ext. etc.) with two (three, four, etc.) 10 mL (or other voL) portions H20 (or other solv.)" mean that the operation is to be performed with indicated vol. of solv. and repeated with same vol. of solv. until number of portions required have been used. (23) Definitions of terms used in methods involving spectro- photometry are those given in JAOAC 37, 54(1954). Most important principles and definitions are: (a) More accurate instrument may be substituted for less accurate instrument (e.g., spectrophtr may replace colorimeter) where latter is specified in method. Wavelength specified in method is understood to be that of max. absorbance (A). unless no peak is present. (b) Absorbance(s) (A).-Neg. logarithm to base 10 of ratio of transmittance (T) of sample to that of ref. or std material. Other xvi names that have been used for quantity represented by this term are optical density, extinction, and absorbancy. (e) Absorptivity(ies) (a).-Absorbance per unit concn and cell length. a = A/be, where b is in cm and c in gil, or a = (A/be) x 1000, if c is in mg/L. Other names that have been used for this or related quantities are extinction coefficient, specific absorption, absorbance index, and £16';'". (d) Transmittance(s) (T).-Ratio of radiant power transmitted by sample to radiant power incident on sample, when both are measured at same spectral position and with same slit width. Beam is understood to be parallel radiation and incident at right angles to plane parallel surface of sample. If sample is soln, solute transmittance is quantity usually desired and is detd directly as ratio of transmittance of soln in cell to transmittance of solv. in an equal cell. Other names that have been used for this quantity are transmittancy and transmission. (e) Standardization.-Spectrophtr may be checked for accu- racy of wavelength scale by ref. to Hg lines: 239.95, 248.3, 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 consistency of absorbance scale, prep. soln of 0.0400 g K2CrO./L 0.05N KOH and det. absorbance at following wavelengths in 1 cm cell: 230 nm, 0.171; 275,0.757; 313.2,0.043; 375, 0.991; 400, 0.396. See "Standards for Checking the Calibration of Spectrophotome- ters," Letter Circular LC-l017, reissued Jan 1967, NBS. (24) Least square treatment of data and calculation of regres- sion lines.-This technic finds the best fitting straight line for set of data such as std curve. It calcs that straight line whose sum of squares of vertical deviations (usually A) of observations from the line is smaller than corresponding sum of squares of deviations from any other line. Equation of straight line is: Y = a + bX, where a is intercept at Y axis (X = 0). and b is slope of line. Least square estimates of constants are: b = I (X, Y,) - [(IX,I Y,)/n] IXf - (IX,)2/n a=Y-bX, where I = "sum of" the n individual values of indicated operation, and X and Yare the averages of the X and Y points. Example: To find "best" straight line relating A (Y) to concn (X): Observation Concn Absorbance No. CI X, Y, X~ X,V, 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 Totals: n=7 IX, = 240 IY, = 3.92 IXl = 13000 I(X,Y,) = 212.1 x= IX,!n = 240/7 = 34.29 Y = IY,!n = 3.92/7 = 0.56 b = 212.1 - (240)(3.92)/7 77.7 = 0.0163 13000 - (240)2/7 4771 a = 0.56 - 0.0163(34.29) = 0.001 Best equation is then: Y = 0.00 + 0.0163X If for sample, A = 0.82, corresponding concn (X) would be: X = (Y - 0.00)/0.0163 =0.82/0.0163 = 50.3.
  18. 18. Many scientific and statistical calculators are preprogrammed to perform this calcn. (25) Common safety precautions are given in Chapter 51. Editorial Conventions (26) For sake of simplicity, abbreviations CI and I instead of CI2 and 12 are used for chlorine and iodine. Similar abbreviations have been used in other cases (0, N, H). The same abbreviation may also be used for the ion where no ambiguity will result. (27) Reagents and app. referenced with only a letter, e.g., (c). will be found in the reagent or apparatus section of that method. (28) To conserve space, most of the articles and some prep- ositions have been eliminated. (29) Names and addresses of manufacturers and suppliers, and trade names of frequently mentioned materials, are fur- nished below solely as a matter of identification and conven- ience, without implication of approval, endorsement, or certifi- cation. The same products available from other suppliers or other brands from other sources may serve equally well if proper tests indicate their use is satisfactory. These firms when mentioned in a method are given by name only (without addresses). Manufacturers and Suppliers Ace Glass, Inc., PO Box 688, 1430 N West Blvd, Vineland, NJ 08360 Aldrich Chemical Co., Inc., 940 W St. Paul Ave, Milwaukee, WI 53233 Allied Chemical Corp., Specialty Chemicals Div., PO Box 1087R, Morristown, NJ 07960 Aluminum Company of America, 1501 Alcoa Bldg, Pittsburgh, PA 15219 American Cyanamid Co., Agricultural Div., PO Box 400, Princeton, NJ 08540 American Instrument Co., Div. of Travenol Laboratories, Inc., 8030 Georgia Ave, Silver Spring, MD 20910 (ASBC) American Society of Brewing Chemists, 3340 Pilot Knob Rd, St. Paul, MN 55121 (ATCC) American Type Culture Collection, 12301 Parklawn Dr, Rockville, MD 20852 Analabs Inc., 80 Republic Dr, North Haven, CT 06473 Applied Science Laboratories, Inc. (Applied Science Division, Milton Roy Co.). PO Box 440, State College, PA 16801 Baird-Atomic, Inc., 125 Middlesex Tnpk, Bedford, MA 01730 J. T. Baker Chemical Co., 222 Red School Ln, Phillipsburg, NJ 08865 Barber-Colman Co., see Searle Analytic, Inc. Bausch & Lomb, Inc., Analytical Systems Div., 820 Linden Ave, Rochester, NY 14625 BBL, Div. of Bioquest, PO Box 243, Cockeysville, MD 21030 Beckman Instruments, Inc., 2500 Harbor Blvd, Fullerton, CA 92634 Becton, Dickinson, & Co., Rutherford, NJ 07070 Bio-Rad Laboratories, 32nd and Griffin Ave, Richmond, CA 94804 Brinkmann Instruments, Inc., Cantiague Rd, Westbury, NY 11590 Burdick & Jackson Laboratories, Inc., 1953 S Harvey St, Muske- gon, MI 49442 Burrell Corp., 2223 Fifth Ave, Pittsburgh, PA 15219 Calbiochem, 10933 N Torrey Pines Rd, La Jolla, CA 92037 Carborundum Co., PO Box 423, Niagara Falls, NY 14302 Cenco Inc., 2600 5 Kostner Ave, Chicago, IL 60623 Coleman Instruments Division, Perkin-Elmer Corp., 2000 York Rd, Oak Brook, IL 60521 Corning Glass Works, Laboratory Products Dept., Corning, NY 14830 xvii Curtin Matheson Scientific, Inc., PO Box 1546, Houston, TX 77001 Ddco Laboratories, PO Box 1058A, Detroit, MI 48232 Dohrmann Div. of Envirotech Corp., 3240 Scott Blvd, Santa Clara, CA 95050 Dow Chemical Co., Ag-Organics Dept., PO Box 1706, Midland, MI48640 Dow Corning Corp., Midland, MI 48640 E. I. du Pont de Nemours & Co., Wilmington, DE 19898 Eastman Kodak Co., Eastman Organic Chemicals, 343 State St, Rochester, NY 14650 Eaton-Dikeman Co., Mt. Holly Springs, PA 17065 Elanco Products Co., Div. of Eli Lilly Co., Elanco Analytical Laboratory, Dept. MC757, Indianapolis, IN 46206 Fisher & Porter Co., Lab Crest Scientific Div., County Line Rd, Warminster, PA 18974 Fisher Scientific Co., 711 Forbes Ave, Pittsburgh, PA 15219 Floridin Co., Berkeley Springs, WV 25411 Foss America Inc., PO Box 504, Route 82, Fishkill, NY 12524 GAF Corp., 140 W 51st St, New York, NY 10020 G.B. Fermentation Industries, Inc., 1 N Broadway, Des Plaines, IL 60016 Geigy Chemical Corp., Saw Mill River Rd, Ardsley, NY 10502 Hamilton Co., PO Box 17500, Reno NV 89510 Hess & Clark Laboratories, Div. of Rhodia, Inc., 7th and Orange Sts, Ashland, OH 44805 Hewlett-Packard Co., 1501 Page Mill Rd, Palo Alto, CA 94304 Hoffman-La Roche, Inc., Nutley, NJ 07110 ICI-America, Inc., Chemical Research Dept., Wilmington, DE 19899 ICN-K&K Laboratories, Inc., 121 Express St, Plainview, NY 11803 ICN Pharmaceuticals, Inc., Life Sciences Group, 26201 Miles Rd, Cleveland, OH 44128 johns-Manville Products Corp., Greenwood Plaza, Denver, CO 80217 Kimble Products, Owens-Illinois, PO Box 1035, Toledo, OH 43666 Kontes Glass Co., Spruce St, Vineland, NJ 08360 Labconco Corp., 8811 Prospect Ave, Kansas City, MO 64132 Eli Lilly & Co., 740 5 Alabama St, Indianapolis, IN 46206 Mallinckrodt Chemicals Works, Science Products Div., 2nd & Mallinckrodt Sts, St. Louis, MO 63147 MC/B Manufacturing Chemists, 2909 Highland Ave, Norwood, OH 45212 Matheson Scientific, Inc., see Curtin Matheson Scientific, Inc. Merck & Co., Inc., 126 E Lincoln Ave, Rahway, NJ 07065 Miles Laboratories, Inc., Elkhart, IN 46514 Monsanto Chemical Co., 800 N Lindberg Blvd, St. Louis, MO 63166 (NBS) National Bureau of Standards, Washington, DC 20234 (NF) National Formulary, see USP New York Laboratory Supply Co., 510 Hempstead Tnpk, West Hempstead, NY 11552 Orion Research Inc., 380 Putnam Ave, Cambridge, MA 02139 Perkin-Elmer Corp., 702-G Main Ave, Norwalk, CT 06856 Phillips Chemical Co., Division of Phillips Petroleum Co., Spe- cialty Chemicals, Drawer '0', Borger, TX 79007. Pierce Chemical Co., PO Box 117, Rockford, IL 61105 H. Reeve Angel & Co., Inc., 9 Bridewell PI, Clifton, NJ 07014 Rohm & Haas Co., Independence Mall West, Philadelphia, PA 19105 Salsbury Laboratories, Charles City, IA 50616 Sargent-Welch Scientific Co., 7300 N Linder Ave, Skokie, IL 60076 (S&S) Schleicher & Schuell, Inc., 543 Washington St, Keene, NH 03431
  19. 19. Schoeffellnstrument Corp., 24 Booker St, Westwood, NJ 07675 SGA Scientific, Inc., 735 Broad St, Bloomfield, NJ 07003 Scientific Products, Div. of American Hospital Supply Corp., 1430 Waukegan Rd, McGaw Park, IL 60085 Searle Analytic, Inc., 2000 Nuclear Dr, Des Plaines, IL 60018 Shell Oil Co., PO Box 2463, Houston, TX 77001 Sigma Chemical Co., PO Box 14508, Sl. Louis, MO 63178 G. Frederick Smith Chemical Co., PO Box 23344, Columbus, OH 43223 Sterwin Chemicals, Inc., 90 Park Ave, New York, NY 10016 Supelco, Bellefonte, PA 16823 Technicon Instruments Corp., 511 Benedict Ave, Tarrytown, NY 10591 Arthur H. Thomas Co., Vine St at 3rd, PO Box 779, Philadelphia, PA 19105 Ultra-Violet Products, Inc., 5100 Walnut Grove Ave, San Gabriel, CA 91778 Union Carbide Corp., Chemicals and Plastics, 270 Park Ave, New York, NY 10017 Union Carbide Corp., Agricultural Products and Services, PO Box 1906, Salinas, CA 93901 Uniroyal Chemical, Elm St, Naugatuck, CT 06770 The Upjohn Co., Kalamazoo, MI 49001 (USDA) U.S. Department of Agriculture, Office of Information, Washington, DC 20250 (USP) United States PharmacopeiaI Convention, Inc., 12601 Twinbrook Pkwy, Rockville, MD 20852 Varian Aerograph, 2700 Mitchell Dr, Walnut Creek, CA 94598 Varian Instrument Div., 611 Hansen Way, Palo Alto. CA 94303 Velsicol Chemical Corp., 341 E Ohio St, Chicago, IL 60611 VWR Scientific, PO Box 3200, San Francisco, CA 94119 Wallerstein Co., see G. B. Fermentation Industries, Inc. Waters Associates, Inc., Maple St, Milford, MA 01757 Winthrop Laboratories, Special Chemicals Dept., 90 Park Ave, New York, NY 10016 Trade Names Amberlite. Ion exchange resins. Rohm and Haas Co. Anakrom. Gas chromatography supports. Analabs, Inc. Celite. Diatomaceous products. Johns-Manville Products Corp. Chromosorb. Chromatographic supports and packings. Johns- Manville Products Corp. Dowex. Ion exchange resins. Dow Chemical Co. Florisil. Chromatographic adsorbents. Floridin Co. Gas-Chrom. Gas chromatography solid supports. Applied Sci- ence Laboratories, Inc. Hyf/o Super-Cel. Diatomaceous products. Johns-Manville Prod- ucts Corp. Skellysolve. Hydrocarbon solvents. Getty Refining and Market- ing Co., PO Box 1650, Tulsa, OK 74102 Tef/on. Chemically resistant polytetrafluoroethylene. E. I. du Pont de Nemours & Co. Tygon. Halogenated vinyl plastic. Norton Co., Plastics & Syn- thetics Div., 12 E Ave, Tallmadge, OH 44278 (30) The foillowing abbreviations, many of which conform with those of Chemical Abstracts, are used. In general, principle governing use of periods after abbreviations is that period is used where final letter of abbreviation is not the same as final letter of word it represents. Periods are not used with units, except inch(es) and gallon(s). xviii Abbreviation a A AA Ac ACS addn addnl alc. alk. alky amp amt anal. anhyd. AOCS app. approx. aq. ASTM atm. avo Be. bp Bu C ca calc. calcd calcg calcn Cat. No. centrf. centrfd centrfg Chap. chern. chromatgc chromatgd chromatgy Ci CI CIPAC cm compd com. conc. concd concg concn const contg cP cpm cryst. crystd crystg crystn cu in. dc del. detd Word absorptivity(ies) absorbance(s) thruout (not restricted to for- mulas); not absorption. A' is used for std; Ao for blank; 3 digit subscript numerals usually denote wavelengths in nm atomic absorption CH3CO- (acetyl, not acetate) American Chemical Society addition additional alcoholic (not alcohol) alkaline (not alkali) alkalinity ampere(s) amount analytical(ly) anhydrous American Oil Chemists' Society apparatus approximate(ly) aqueous American Society for Testing and Materials atmosphere, atmospheric average (except as verb) degree Baume boiling point butyl degrees Celsius (Centigrade) about, approximately calculate calculated calculating calculation Catalog Number centrifuge centrifuged centrifuging Chapter chemical(ly) chromatographic chromatographed chromatography curie(s) Color Index Collaborative International Pesticides Ana- lytical Council centimeter(s) compound commercial(ly) concentrate (as verb or noun) concentrated concentrating concentration constant containing centipoise counts per minute crystalline (not crystallize) crystallized crystallizing crystallization cubic inch(es) direct current determine determined
  20. 20. Abbreviation detg detn diam. diat. earth dil. dild dilg diln distd distg distn DMF DMSO EDTA e.g. elec. equiv. est. estd estg estn Et EtOH evap. evapd evapg evapn ext extd extg extn F FAO Fig. fl oz fp ft g g gal. GLC g-s HCHO HOAc HPLC hr ht id in. inorg. insol. IR ISO JAOAC kg L Ib liq. m Word determining determination diameter diatomaceous earth dilute diluted diluting dilution distilled distilling distillation N,N-dimethylformamide dimethyl sulfoxide ethylenedinitrilotetraacetic acid (or -tetra- acetate) for example electric(al) equivalent estimate estimated estimating estimation ethyl ethanol (the chemical entity C2H50H) evaporate evaporated evaporating evaporation extract extracted extracting extraction degrees Fahrenheit (DC = (5/9) x (OF - 32)) Food and Agriculture Organization Figure (illustration) fluid ounce(s) (29.57 mL) freezing point foot (30.48 cm) gram(s) gravity (in centrfg) gallon(s) (3.785 L) gas-liquid chromatography glass-stoppered formaldehyde acetic acid (not HAc) high pressure (or performance) liquid chro- matography hourIs) height inner diameter (or dimension) inch(es) (2.54 cm) inorganic insoluble infrared International Organization for Standardiza- tion Journal of the Association of Official Analyt- ical Chemists (after 1965) Journal of the Association of Official Agri- cultural Chemists (before 1966) kilogram(s) liter(s) pound(s) (453.6 g) liquid meter(s); milli-as prefix xix Abbreviation m M ma mag. max. mech. Me MeOH mg min min. mixt. mL mm mp mIL mv MW N N n NBS NCA neg. neut. neutze neutzd neutzg neutzn NF ng nm No. -OAc_ -OCN od org. oxidn oz p Pa par. pet ether phthln pos. powd ppb ppm ppt pptd pptg pptn Pr prep. prepd prepg prepn psi psig pt Word molal molar (as applied to concn). not molal milliampere (et amp) magnetic(ally) maximum mechanical(ly) methyl methyl alcohol milligram(s) minute(s) minimum mixture milliliter(s) millimeter(s) melting point millimicron (10-6 mm); use nanometer (nm) (10-9 m) millivolt molecular weight normal (as applied to concn); in equations. normality of titrating reagent Newton (105 dynes) refractive index National Bureau of Standards National Canners Association (now National Food Processors Associa.tion) negative neutral neutralize neutralized neutralizing neutralization National Formulary nanogram (10-9 g) nanometer (10-9 m); formerly mIL number acetate (cf Ac) cyanate outer diameter (or dimension) organic oxidation ounce(s) (28.35 g) pico (10-12 ) as prefix Pascal (1 Newton/m2 ; 9.87 x 10-6 atm.; 7.5 x 10-3 mm Hg (torr); 1.45 x 10--4 psi) paragraph(s) petroleum ether phenolphthalein positive powdered (as adjective) parts per billion (1/109 ) parts per million (1/106 ) preci pitate precipitated precipitating precipitation propyl prepare prepared preparing preparation pounds per square inch (absolute) pounds per square inch gage (atmospheric pressure = 0) pint(s) (473 mL)

×