Page:NIOSH Manual of Analytical Methods - 5601.pdf/1

 ORGANONITROGEN PESTICIDES

FORMULAE: Figure 1

MW: Table 1

METHOD: 5601, Issue 1

OSHA : NIOSH: ACGIH:

CAS: Table 1

EVALUATION: FULL

Table 1 Table 1 Table 1 (Table 1) Aldicarb Benomyl Chlorprophan Diuron Propham Propoxur

Captan Formetanate Thiobencarb

Table 1

Carbaryl Carbendazim Methiocarb Methomyl

SAMPLING SAMPLER:

RTECS: Table 1

Issue 1: 15 January 1998

PROPERTIES:

NAMES and SYNONYMS:

5601

Carbofuran Oxamyl

MEASUREMENT

FILTER/SOLID SORBENT TUBE (OVS-2 Tube: 13-mm quartz fiber filter; XAD-2, 270 mg/140 mg)

TECHNIQUE:

HPLC, UV detection

ANALYTE:

organonitrogen pesticides (Table 1)

FLOW RATE:

0.1 to 1 L/min [1]

EXTRACTION:

VOL-MIN: -MAX:

variable (see Table 2) 480 L

2 mL extraction solution (0.2% V/V 0.1 M aqueous triethylamine phosphate buffer in acetonitrile, pH 6.9 to 7.1)

SHIPMENT:

routine

INJECTION VOLUME:

SAMPLE STABILITY:

BLANKS:

at least 30 days @ -12 C [1] at least 7 days @ 24 C [1]

5 µL

MOBILE PHASE A: 2% 1-propanol in aqueous 0.02 M triethylamine phosphate (pH 6.9 to 7.1) MOBILE PHASE B: 2% 1-propanol in acetonitrile PROGRAM:

mobile phase B, 3 to 95% in 30 min, hold 95% 5 min

COLUMN:

NOVA-PAK® C-18, 30 cm x 3.9-mm ID, or equivalent; ambient temperature (Table 3)

2 to 10 field blanks per set

ACCURACY RANGE STUDIED:

Table 2

DETECTOR:

UV absorption at 200 and 225 nm

BIAS:

Table 2

CALIBRATION:

solutions of analytes in extraction fluid

RANGE:

Table 2

OVERALL PRECISION ( ACCURACY:

rT

): Table 2 Table 2

ESTIMATED LOD: Table 2 PRECISION ( r):

Table 2

APPLICABILITY: The working ranges (Table 2) for aldicarb, carbofuran, and oxamyl range from 0.5 to 10 times the OSHA PEL. Others cover 0.1 to 2 times the OSHA PELs with appropriate dilutions [1].This method may be applicable to the determination of other organonitrogen compounds after evaluation, and to a broad range of pesticides having UV chromophores, e.g., acetanilides, acid herbicides, organophosphates, phenols, pyrethroids, sulfonyl ureas, sulfonamides, triazines, and uracil pesticides.

INTERFERENCES: Because of the broad response of the UV detector at shorter wavelengths, there are many potential interferences. Those tested include solvents (chloroform and toluene), antioxidants (BHT), plasticizers (dialkyl phthalates), nitrogen compounds (nicotine and caffeine), impurities in HPLC reagents (e.g., in triethylamine), other pesticides (2,4-D, atrazine, parathion, etc.), and pesticide hydrolysis products (1-naphthol). Retention times are given in Table 4. Confirmation techniques are recommended when analyte identity is uncertain.

OTHER METHODS: This method may be used to replace previous related pesticide methods: S273 Carbaryl [2]; 5006 Carbaryl [3]; OSHA 63 Carbaryl and 74 Aldicarb [4]; OSHA Stopgap methods for several pesticides [5]; and EPA TO-10 for captan, Folpet, and Mexacarbate [6]. The OVS-2 Tube is similar in concept to the device of Hill and Arnold [7], but offers convenience and lower flow resistance.

NIOSH Manual of Analytical Methods, Fourth Edition