Page:NIOSH Manual of Analytical Methods - 5008.pdf/1

 PYRETHRUM

C20 H28 O3 to C22 H30 O5

MW: 316.4 to 372.4

(Table 1)

5008

CAS: 8003-34-7

RTECS: UR4200000

(active constituents)

METHOD: 5008, Issue 2

EVALUATION: FULL

OSHA : 5 mg/m 3 NIOSH: 5 mg/m 3; Group II pesticide ACGIH: 5 mg/m 3

PROPERTIES:

Issue 1: 15 May 1985 Issue 2: 15 August 1994

viscous brown resin or solid; VP not significant

SYNONYMS: Active constituents include pyrethrin I and II, jasmolin I and II, and cinerin I and II.

SAMPLING

MEASUREMENT

SAMPLER:

FILTER (glass fiber)

TECHNIQUE:

HPLC, UV DETECTION

FLOW RATE:

1 to 4 L/min

ANALYTE:

six active constituents of pyrethrum

VOL-MIN: -MAX:

20 L 400 L

EXTRACTION:

10 mL acetonitrile; stand 30 min

SHIPMENT:

routine; ship bulk sample separately

INJECTION VOLUME:

25 µL

SAMPLE STABILITY:

FIELD BLANKS:

COLUMN:

C 18 reverse phase, 10-µm packing, 25 to 30 cm

MOBILE PHASE:

85% acetonitrile/15% water, isocratic, 1.0 mL/min, room temperature, 2800 kPa (400 psi)

DETECTOR:

UV absorption @ 225 nm

CALIBRATION:

solutions of pyrethrum in acetonitrile

RANGE:

0.1 to 1.8 mg per sample

at least 1 week @ 25 °C [1]

2 to 10 field blanks per set

ACCURACY 3

RANGE STUDIED:

1.4 to 8.5 mg/m [1] (132-L samples)

BIAS:

- 4.5% ESTIMATED LOD: 0.01 mg per sample

ˆ rT): 0.070 [1] OVERALL PRECISION (S PRECISION (Sr): ACCURACY:

0.040 [1]

± 13.8%

APPLICABILITY: The working range is 0.5 to 10 mg/m 3 for a 200-L air sample.

INTERFERENCES: Specific interferences have not been studied. Mass spectrometry or gas-liquid chromatography with electron-capture detection may be needed for confirmation [1].

OTHER METHODS: This method is S298 [2] in a revised format. For bulk samples, gas-liquid chromatography with electron-capture detection has been recommended [3]. A modified HPLC method (C 8 column, programmed methanol/water or acetonitrile, isocratic) has been used [4].

NIOSH Manual of Analytical Methods (NMAM), Fourth Edition, 8/15/94