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
