Page:NIOSH Manual of Analytical Methods - 9200.pdf/1

 CHLORINATED AND ORGANONITROGEN HERBICIDES (HAND WASH)

ANALYTES: Figure 1 Formula: Table 1 METHOD: 9200, Issue 1

OSHA: NIOSH: ACGIH: NAMES:

MW: Table 1

CAS: Table 1

EVALUATION: PARTIAL

Table 1 Table 1 Table 1

SHIPMENT:

Alachlor Cyanazine

Atrazine Metolachlor

Simazine 2,4-D acid

POLYETHYLENE BAG 12" x 18", polyethylene bag containing 150 mL isopropanol

transfer wash to 250-mL wide-mouthed glass jars with PTFE-lined caps.

Issue 1: 15 January 1998

2,4-D, 2-ethylhexyl ester 2,4-D, 2-butoxyethyl ester

MEASUREMENT TECHNIQUE:

GAS CHROMATOGRAPHY/ ELECTRON CAPTURE (GC/ECD)

ANALYTE: INJECTION VOLUME:

listed above or Table 1 2 µL

TEMPERATURE-INJECTION: -DETECTOR: -COLUMN:

SAMPLE STABILITY:

at least 30 days at 5 °C [1]

BLANKS:

2 to 10 field blanks per set

ACCURACY

He at 1 mL/min

COLUMN:

capillary, fused silica, 30 m X 0.25-mm ID, 0.25-µm film, 50% phenyl, 50% methyl silicone, DB-17 or equivalent. See Table 2

CALIBRATION:

standard solutions isopropanol Table 3

not studied

ACCURACY:

not determined

BIAS:

not determined

RANGE:

not determined

ESTIMATED LOD: Table 3

rT

):

270 C 300 C 90 C for 1 min; ramp to 160 C at 35 C/min; then ramp to 230 C at 3 C/min; hold for 9 min.

CARRIER GAS:

RANGE STUDIED:

OVERALL PRECISION (

RTECS: Table 1

PROPERTIES: Table 1

SAMPLING SAMPLER:

9200

PRECISION ( r):

of

herbicides

in

Table 3

APPLICABILITY: The working ranges are listed in Table 3. These cover from the LOQ to approximately 30 x LOQ. This method may be applicable to the determination of many other thermally stable organonitrogen, aryl and alkyl acidic, and phenolic pesticides after evaluation for sample stability and precision.

INTERFERENCES: Because of the great sensitivity of the ECD, there are many potential interferences. Among those observed are plasticizers (e.g., dibutyl phthalate), methylated fatty acids (give negative responses), phenols, and antioxidants and other additives (e.g., BHT), any volatile or semivolatile halogenated or nitrated organics, organophosphorous compounds, and other pesticides. Agricultural spray additives can contribute serious interferences. Such additives include solvents, emulsifiers, wetting agents, breakdown products, and fertilizers (e.g., fatty acids and urea). Second-column confirmation is very desirable.

OTHER METHODS: Other hand wash methods allowing simultaneous determination of organonitrogen and acid compounds and their esters are unknown.

NIOSH Manual of Analytical Methods (NMAM), Fourth Edition