Page:NIOSH Manual of Analytical Methods - 5046.pdf/1

 TETRAKIS(HYDROXYMETHYL)PHOSPHONIUM CHLORIDE

P(CH2 OH)4 + C1–

MW: 190.58

METHOD: 5046, Issue 1

EVALUATION: PARTIAL

OSHA: None NIOSH: None ACGIH: None

SYNONYMS:

CAS: 124-64-1

PROPERTIES:

RTECS: TA2450000 Issue 1: 15 March 2003

hygroscopic, air sensitive solid; MP 151 o C; ionic; does not vaporize; soluble in water, methanol; insoluble in diethyl ether

tetramethylolphosphonium chloride, tetrahydroxymethylphosphonium chloride, THPC, Pyroset TKC, Proban CC, Retardol C, NCI-C55061, Tolcide THPC

SAMPLING SAMPLER:

5046

37-mm filter cassette (open-faced cassette containing two glass fiber filters coated with acidified 2,4-dinitrophenylhydrazine)

MEASUREMENT TECHNIQUE:

HPLC; UV DETECTION

ANALYTE:

2,4-dinitrophenylhydrazone of formaldehyde

EXTRACTION:

4 mL acetonitrile; 60 o C, 1 hour

INJECTION VOLUME:

20 :L

MOBILE PHASE:

45:55 acetonitrile:water @ 1.3 mL/min

COLUMN:

3.9 x 150 mm stainless steel, packed with 5-µm C-18, SymmetryT M or equivalent

DETECTOR:

UV @ 360 nm

CALIBRATION:

DNPH-coated glass fiber filters fortified with THPC (media standards)

RANGE:

6.5 to 60 µg/sample (instrumental)[1]

ESTIMATED LOD:

2 µg/sample

PRECISION (S r ):

0.0585 for 8 to 31 µg per sample

FLOW RATE: 1.0 to 1.7 L/min 3

VOL-MIN: -MAX:

1 L @ 6.5 mg/m 480 L @ 0.15 mg/m3

SHIPMENT:

Ship on ice (0 o C).

SAMPLE STABILITY: BLANKS:

28 days @ 5 o C [1] 2 to 10 field blanks per set 10 media blanks per set ACCURACY

RANGE STUDIED:

Not studied

BIAS:

Not determined

OVERALL PRECISION ( Ö r T ):

Not determined

ACCURACY:

Not determined

APPLICABILITY: The theoretical working range is 0.43 to about 67 mg/m3 for a 15-L air sample. This method may be applicable to other tetrakis(hydroxymethyl)phosphonium salts, such as the sulfate. However, evaluation of this method has been limited to THPC. INTERFERENCES: Formaldehyde gas is an interference. Concentrations of THPC can be corrected for formaldehyde gas by sampling for formaldehyde gas with NMAM 2016 [2]. Ozone has been observed to consume DNPH and to degrade the DNPH derivative of formaldehyde [3]. However, use of an ozone scrubber is not recommended because this scrubber may trap THPC aerosol. Ketones and other aldehydes can react with DNPH; the derivatives produced, however, are separated chromatographically from the analyte of interest. OTHER METHODS: Other methods for THPC in air are unknown. A microanalytical method for tetrakis(hydroxymethyl) phosphonium salts in solution involves ion chromatography, post-column reaction with an acetylacetone reagent to form a formaldehyde derivative, and detection at 425 nm [4].

NIOSH Manual of Analytical Methods (NMAM), Fourth Edition