National Institute for Occupational Safety and Health

Name: NIOSH Manual of Analytical Methods — Chlorinated and Organonitrogen Herbicides (Air Sampling) (5602)
Author: National Institute for Occupational Safety and Health

NIOSH Manual of Analytical Methods… (1994)

Summary

“NIOSH Manual of Analytical Methods — Chlorinated and Organonitrogen Herbicides (Air Sampling) (5602)”, published in 1994, is a work by National Institute for Occupational Safety and Health. It explores elements such as Fourth Edition CHLORINATED, diazomethane and analyte.

Quotes from NIOSH Manual of Analytical Methods… (National Institute for Occupational Safety and Health)

National Institute for Occupational Safety and Health, NIOSH Manual of Analytical Methods… (1994)

“ If primary analysis was performed using a nonpolar or weakly polar column (e.g., DB-1 or DB-5) confirmation should be accomplished by reanalysis on a polar columne.g., ( DB-17 or DB-1701) . See Table 4 for approximate retention times for each column type. For positive identification of high-level analytes (1 to 10 μg/mL or greater) , GC/MS may be used. Figure 4 shows a typical chromatogram using a DB-17 column. Figure 5 shows a typical chromatogram using a DB-5 column. Table 5 gives notes on the analytical characteristics of the chlorinated organonitrogen and acid herbicides. ”

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Source: Wikisource

National Institute for Occupational Safety and Health, NIOSH Manual of Analytical Methods… (1994)

“ Average recovery for individual pesticides on Day 1 was 110 to 120% with cyanazine having a high recovery of 150% and 2,4-D acid having a recovery of 91%. Day 30 storage samples had a range of recoveries from 70 to 82% based on Day 1, with 2,4-D acid and simazine having recoveries of 104% and 88%, respectively. Day 50 samples had average recoveries of 80% of Day 1, with 2,4-D acid having 101 % recovery, and cyanazine having a 69% recovery.
REFERENCES: [1] [2]
[3]
[4] [5]
NIOSH [1995] . Back-up data report for chlorinated organonitrogen and carboxylic acid herbicides. ”

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Source: Wikisource

National Institute for Occupational Safety and Health, NIOSH Manual of Analytical Methods… (1994)

“ The analytical conditions used in the evaluation are in Table 4 with the DB-5ms column. The front filter of each sample tube was fortified with an aliquot of a solution containing the 8 herbicides. Air was then drawn through the tubes at 1 L/min for 8 h (480 Ltotal volume) at 30 °C. One set of samplers was tested at 15% relative humidity (RH) and the other set was tested at 80% RH. All samples were stored at 4C. Humidity did not affect the analyte recoveries from the samplers. A long-term storage study also was done. ”

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Source: Wikisource

National Institute for Occupational Safety and Health, NIOSH Manual of Analytical Methods… (1994)

“ Add 10 mg silicic acid to each standard vial, and let stand for an additional hour. c. Filter through a 0.45-μm syringe filter into a GC vial. d. Analyze together with field samples and blanks (steps 12 and 13) . e. Prepare calibration graph (peak area or height vs. μg analyte) . 10. Determine desorption efficiency (DE) at least once for each lot of OVS tubes used for sampling. Independently prepared quality control herbicide solutions in extraction solvent must be prepared at concentrationswithin the analytical range. Prepare three samplers at each of six levels plus three media blanks. ”

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Source: Wikisource

National Institute for Occupational Safety and Health, NIOSH Manual of Analytical Methods… (1994)

“ The resulting diazomethane gas is swept by a flow of nitrogen gas into a flask of chilled (0 °C) methyl t-butyl ether/methanol extraction solvent (maximum volume, 500 mL) . NOTE: KOH solution (37% w/v) will become weaker over time owing to adsorption of atmospheric carbon dioxide. Under such circumstances, diazomethane generation will be considerably slower.
NIOSH Manual of Analytical Methods (NMAM) , Fourth Edition CHLORINATED AND ORGANONITROGEN HERBICIDES (AIR SAMPLING) : METHOD 5602, Issue 1, dated 15 January 1998 - Page 6 of 14
TABLE 1. ”

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Source: Wikisource

National Institute for Occupational Safety and Health, NIOSH Manual of Analytical Methods… (1994)

“ Because of the great sensitivity of the ECD, there are many potential interferences. Those observed are plasticizers (e.g., dibutyl phthalate) , methylated fatty acids (negative response) , phenols, antioxidants, and other additives (e.g., BHT) , any volatile or semivolatile halogenated or nitrated organic, organophosphorous compounds, and other pesticides. ”

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Source: Wikisource

National Institute for Occupational Safety and Health, NIOSH Manual of Analytical Methods… (1994)

“ Syringe, luer lock, 1-, 2.5-, or 5-mL, for sample filtering. Platform shaker
SPECIAL PRECAUTIONS: Diazomethane has been cited as a carcinogen. It is extremely toxic and highly irritating. Diazomethane may explode under some conditions. Do not heat above 90 °C. Avoid rough surfaces: fire-polish glass tubing, or use Teflon®. Do not expose solutions to strong light. Keep dilute solutions at 0 °C. Prepare in a hood [5] . Avoid skin contact withDiazald® and herbicides. Avoid skin contact and open flame with solvents. ”

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Source: Wikisource

National Institute for Occupational Safety and Health, NIOSH Manual of Analytical Methods… (1994)

“ D i a z a l d® ( N - m e t h y l - N - n i t r o s o p-toluenesulfonamide.) * Silicic Acid, 100-mesh. Diazomethane* derivatizing reagent. (See APPENDIX) Herbicide stock solutions. Prepare individual standard stock solutions of each herbicide of interest in extraction solvent. NOTE: All herbicides in Table 1 were found to be soluble to at least 1 mg/mL, except simazine, which is soluble to 0.5 mg/mL. Calibration stock solution. Dilute the appropriate volume of herbicide stock solution to a known volume with extraction solvent. NOTE: Spiking solutions may contain more than one analyte. ”

National Institute for Occupational Safety and Health

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Quotes from NIOSH Manual of Analytical Methods… (National Institute for Occupational Safety and Health)

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