Loading (50 kb)...'
(continued) m/z 198.
441.......................... 44 to 110% of m/z 443.
442.......................... 30 to 86% of m/z 198.
443.......................... 14 to 24% of m/z 442.
------------------------------------------------------------------------
\1\ Reference 7.
Table 4_Characteristic M/Z's of Chlorophenolic Compounds
------------------------------------------------------------------------
Compound Primary m/z
------------------------------------------------------------------------
4-chlorophenol.......................................... 128
2,4-dichlorophenol...................................... 162
2,4-dichlorophenol-d3................................... 167
2,6-dichlorophenol...................................... 162
2,4,5-trichlorophenol................................... 196
2,4,6-trichlorophenol................................... 196
2,3,4,6-tetrachlorophenol............................... 232
pentachlorophenol....................................... 266
pentachlorophenol-13C6.................................. 272
4-chloroguaiacol........................................ 158
4-chloroguaiacol-13C6................................... 164
3,4-dichloroguaiacol.................................... 192
4,5-dichloroguaiacol.................................... 192
4,6-dichloroguaiacol.................................... 192
3,4,5-trichloroguaiacol................................. 226
3,4,6-trichloroguaiacol................................. 226
4,5,6-trichloroguaiacol................................. 226
4,5,6-trichloroguaiacol-13C6............................ 234
tetrachloroguaiacol..................................... 262
tetrachloroguaiacol-13C6................................ 268
4-chlorocatechol........................................ 144
3,4-dichlorocatechol.................................... 178
3,6-dichlorocatechol.................................... 178
4,5-dichlorocatechol.................................... 178
4,5-dichlorocatechol-13C6............................... 184
3,4,5-trichlorocatechol................................. 212
3,4,6-trichlorocatechol................................. 212
tetrachlorocatechol..................................... 248
tetrachlorocatechol-13C6................................ 254
5-chlorovanillin........................................ 186
5-chlorovanillin-13C6................................... 192
6-chlorovanillin........................................ 186
5,6-dichlorovanillin.................................... 220
2-chlorosyringaldehyde.................................. 216
2,6-dichlorosyringaldehyde.............................. 250
trichlorosyringol....................................... 256
Sample Matrix Internal Standard (SMIS)
3,4,5-trichlorophenol................................... 196
Instrument Internal Standard (IIS)
2,2[prime]-difluorobiphenyl............................. 190
------------------------------------------------------------------------
Table 5_Acceptance Criteria for Performance Tests \1\
----------------------------------------------------------------------------------------------------------------
Initial precision Labeled compound and
and recovery sec. SMIS recovery sec.
Test conc. 9.3.2 (percent) Ongoing 9.4 and 14.6
\3\ ---------------------- recovery ---------------------
EGD No. \2\ Compound (µg/ sec. 9.6 With Without
mL) (percent) ascorbic ascorbic
s X acid P acid P
(%) (%)
----------------------------------------------------------------------------------------------------------------
1001........................ 4-chlorophenol. 25 64 72-144 40-236
1202........................ 2,4- 50 14 84-120 84-118
dichlorophenol.
1102........................ 2,4- 25 54 64-160 56-170 58-135 27-143
dichlorophenol-
d3.
1003........................ 2,6- 50 20 66-148 58-170
dichlorophenol.
1004........................ 2,4,5- 50 14 78-140 82-128
trichloropheno
l.
1005........................ 2,4,6- 50 20 72-142 72-146
trichloropheno
l.
1006........................ 2,3,4,6- 50 14 80-132 82-132
tetrachlorophe
nol.
1207........................ pentachlorophen 100 6 90-111 84-120
ol.
1107........................ pentachlorophen 25 21 58-169 61-157 8-143 27-167
ol-\13\C6.
1208........................ 4- 25 20 88-120 88-120
chloroguaiacol.
1108........................ 4- 25 104 68-148 64-152 59-121 43-168
chloroguaiacol-
\13\C6.
1009........................ 3,4- 50 18 80-126 82-126
dichloroguaiac
o \4\.
1010........................ 4,5- 50 14 82-121 80-128
dichloroguaiac
ol.
1011........................ 4,6- 50 16 82-126 86-120
dichloroguaiac
ol.
1012........................ 3,4,5- 50 16 78-130 80-134
trichloroguaia
col.
1013........................ 3,4,6- 50 16 64-152 74-140
trichloroguaia
col.
1214........................ 4,5,6- 50 14 92-106 88-116
trichloroguaia
col.
1114........................ 4,5,6- 25 48 66-146 74-140 48-131 51-139
trichloroguaia
col-\13\C6.
1215........................ tetrachloroguai 100 7 84-115 81-126
acol.
1115........................ tetrachloroguai 25 22 57-173 65-161 35-120 27-161
acol-\13\C6.
1016........................ 4- 25 48 76-140 80-124
chlorocatechol.
1017........................ 3,4- 50 24 66-154 78-134
dichlorocatech
ol.
1018........................ 3,6- 50 16 78-136 84-126
dichlorocatech
ol.
1219........................ 4,5- 50 8 84-118 86-122
dichlorocatech
ol.
1119........................ 4,5- 25 78 68-144 66-142 33-129 0-190
dichlorocatech
ol-\13\C6.
1020........................ 3,4,5- 100 17 60-166 72-128
trichlorocatec
hol.
1021........................ 3,4,6- 100 17 74-138 64-149
trichlorocatec
hol \4\.
1222........................ tetrachlorocate 100 29 46-234 81-132
chol.
1122........................ tetrachlorocate 25 39 48-227 63-152 14-118 0-184
chol-\13\C6.
1223........................ 5- 50 20 94-208 84-118
chlorovanillin.
1123........................ 5- 25 84 68-160 70-144 51-126 32-254
chlorovanillin-
\13\C6.
1024........................ 6- 50 22 82-128 80-126
chlorovanillin.
1025........................ 5,6- 100 9 67-146 77-140
dichlorovanill
in.
1026........................ 2- 50 28 76-130 72-156
chlorosyringal
dehyde.
1027........................ 2,6- 100 14 82-129 60-183 ......... .........
dichlorosyring
aldehyde.
1028........................ trichlorosyring 50 18 76-136 66-174
ol.
Sample Matrix Internal Standard
----------------------------------------------------------------------------------------------------------------
184......................... 3,4,5- 100 47 62-185 68-144 56-116 24-167
trichloropheno
l.
----------------------------------------------------------------------------------------------------------------
\1\ Specifications derived from multi-laboratory testing of draft method.
\2\ Four-digit numbers beginning with 10 indicate a pollutant quantified by the internal standard method; four-
digit numbers beginning with 11 indicate a labeled compound quantified by the internal standard method; four-
digit numbers beginning with 12 indicate a pollutant quantified by isotope dilution.
\3\ Test concentrations are in units of µg/mL.
\4\ Specification derived from isomer.
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20.0 Glossary of Definitions and Purposes
These definitions and purposes are specific to this method but have been conformed to common usage as much as possible.
20.1 Units of weight and measure and their abbreviations
20.1.1 Symbols.
°C degrees Celsius
µL microliter
< less than
> greater than
% percent
20.1.2 Alphabetical characters.
cm centimeter
g gram
h hour
ID inside diameter
in. inch
L liter
M Molecular ion
m meter
mg milligram
min minute
mL milliliter
mm millimeter
m/z mass-to-charge ratio
N normal; gram molecular weight of solute divided by hydrogen equivalent of solute, per liter of solution
OD outside diameter
pg picogram
ppb part-per-billion
ppm part-per-million
ppt part-per-trillion
psig pounds-per-square inch gauge
v/v volume per unit volume
w/v weight per unit volume
20.2 Definitions and acronyms (in alphabetical order).
Analyte: A chlorophenolic tested for by this method.
The analytes are listed in Table 1.
Calibration standard (CAL): A solution prepared from a secondary standard and/or stock solutions and used to calibrate the response of the instrument with respect to analyte concentration.
Calibration verification standard (VER): The mid-point calibration standard (CS3) that is used to verify calibration. See Table 4.
Chlorophenolics: collectively, the analytes listed in Table 1.
CS1, CS2, CS3, CS4, CS5: See Calibration standards and Table 4.
Field blank: An aliquot of reagent water or other reference matrix that is placed in a sample container in the laboratory or the field, and treated as a sample in all respects, including exposure to sampling site conditions, storage, preservation, and all analytical procedures. The purpose of the field blank is to determine if the field or sample transporting procedures and environments have contaminated the sample.
GC: Gas chromatograph or gas chromatography.
HRGC: High resolution GC.
IPR: Initial precision and recovery; four aliquots of the diluted PAR standard analyzed to establish the ability to generate acceptable precision and accuracy. An IPR is performed prior to the first time this method is used and any time the method or instrumentation is modified.
K-D: Kuderna-Danish concentrator; a device used to concentrate the analytes in a solvent.
Laboratory blank: See Method blank.
Laboratory control sample (LCS): See Ongoing precision and recovery standard (OPR).
Laboratory reagent blank: See Method blank.
May: This action, activity, or procedural step is neither required nor prohibited.
May not: This action, activity, or procedural step is prohibited.
Method blank: An aliquot of reagent water that is treated exactly as a sample including exposure to all glassware, equipment, solvents, reagents, internal standards, and surrogates that are used with samples. The method blank is used to determine if analytes or interferences are present in the laboratory environment, the reagents, or the apparatus.
Minimum level (ML): The level at which the entire analytical system must give a recognizable signal and acceptable calibration point for the analyte. It is equivalent to the concentration of the lowest calibration standard, assuming that all method-specified sample weights, volumes, and cleanup procedures have been employed.
MS: Mass spectrometer or mass spectrometry.
Must: This action, activity, or procedural step is required.
OPR: Ongoing precision and recovery standard (OPR); a laboratory blank spiked with known quantities of analytes. The OPR is analyzed exactly like a sample. Its purpose is to assure that the results produced by the laboratory remain within the limits specified in this method for precision and recovery.
PAR: Precision and recovery standard; secondary standard that is diluted and spiked to form the IPR and OPR.
Preparation blank: See Method blank.
Primary dilution standard: A solution containing the specified analytes that is purchased or prepared from stock solutions and diluted as needed to prepare calibration solutions and other solutions.
Quality control check sample (QCS): A sample containing all or a subset of the analytes at known concentrations. The QCS is obtained from a source external to the laboratory or is prepared from a source of standards different from the source of calibration standards. It is used to check laboratory performance with test materials prepared external to the normal preparation process.
Reagent water: Water demonstrated to be free from the analytes of interest and potentially interfering substances at the method detection limit for the analyte.
Relative standard deviation (RSD): The standard deviation times 100 divided by the mean.
RF: Response factor. See Section 10.5.1.
RR: Relative response. See Section 10.4.4.
RSD: See Relative standard deviation.
Should: This action, activity, or procedural step is suggested but not required.
Stock solution: A solution containing an analyte that is prepared using a reference material traceable to EPA, the National Institute of Science and Technology (NIST), or a source that will attest to the purity and authenticity of the reference material.
VER: See Calibration verification standard.