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    Allyl Chloride 1000: CH CHCH CL MW: 76.53 CAS: 107-05-1 RTECS: UC7350000

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    Luis Trejo
    This document describes a method for sampling and analyzing allyl chloride in air using solid sorbent sampling tubes, gas chromatography with flame ionization detection, and other procedures. Key details include: - Allyl chloride is collected on coconut shell charcoal tubes at 0.01-1 L/min for 16-100 L and desorbed with 1 mL benzene. - Samples are analyzed by GC-FID using temperatures of 185-200°C (injection), 250°C (detector), and 160-200°C (column). - The method was validated over 1.8-7.2 mg/m3 with 6.4% average recovery and 0.071 precision. The

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    Allyl Chloride 1000: CH CHCH CL MW: 76.53 CAS: 107-05-1 RTECS: UC7350000

    Uploaded by

    Luis Trejo
    42 views3 pages
    This document describes a method for sampling and analyzing allyl chloride in air using solid sorbent sampling tubes, gas chromatography with flame ionization detection, and other procedures. Key details include: - Allyl chloride is collected on coconut shell charcoal tubes at 0.01-1 L/min for 16-100 L and desorbed with 1 mL benzene. - Samples are analyzed by GC-FID using temperatures of 185-200°C (injection), 250°C (detector), and 160-200°C (column). - The method was validated over 1.8-7.2 mg/m3 with 6.4% average recovery and 0.071 precision. The

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    This document describes a method for sampling and analyzing allyl chloride in air using solid sorbent sampling tubes, gas chromatography with flame ionization detection, and other procedures. Key details include: - Allyl chloride is collected on coconut shell charcoal tubes at 0.01-1 L/min for 16-100 L and desorbed with 1 mL benzene. - Samples are analyzed by GC-FID using temperatures of 185-200°C (injection), 250°C (detector), and 160-200°C (column). - The method was validated over 1.8-7.2 mg/m3 with 6.4% average recovery and 0.071 precision. The

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    © All Rights Reserved
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    42 views3 pages

    Allyl Chloride 1000: CH CHCH CL MW: 76.53 CAS: 107-05-1 RTECS: UC7350000

    Uploaded by

    Luis Trejo
    This document describes a method for sampling and analyzing allyl chloride in air using solid sorbent sampling tubes, gas chromatography with flame ionization detection, and other procedures. Key details include: - Allyl chloride is collected on coconut shell charcoal tubes at 0.01-1 L/min for 16-100 L and desorbed with 1 mL benzene. - Samples are analyzed by GC-FID using temperatures of 185-200°C (injection), 250°C (detector), and 160-200°C (column). - The method was validated over 1.8-7.2 mg/m3 with 6.4% average recovery and 0.071 precision. The

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    ALLYL CHLORIDE

    1000
    CH2=CHCH2ClMW: 76.53CAS: 107-05-1RTECS: UC7350000
    METHOD: 1000, Issue 2

    EVALUATION: FULL

    OSHA: 1 ppm
    NIOSH: 1 ppm; STEL 2 ppm
    ACGIH: 1 ppm; STEL 2 ppm

    (1 ppm = 3.13 mg/m @ NTP)

    Issue 1: 15 February 1984


    Issue 2: 15 August 1994

    PROPERTIES: liquid; d 0.938 g/mL @ 20 C; BP 45 C; MP


    135 C; VP 39.3 kPA (295 mm Hg) @ 25 C;
    explosive range 3.3 to 11% v/v in air

    SYNONYMS: 3-chloro-1-propene; 1-chloro-2-propene


    SAMPLING
    SAMPLER: SOLID SORBENT TUBE
    (coconut shell charcoal, 100 mg/50 mg)

    MEASUREMENT
    TECHNIQUE:

    GAS CHROMATOGRAPHY, FID

    ANALYTE:

    allyl chloride

    DESORPTION:

    1 mL benzene; stand 30 min

    INJECTION
    VOLUME:

    5 L

    FLOW RATE: 0.01 to 1 L/min


    VOL-MIN:
    -MAX:

    16 L @ 1 ppm
    100 L

    SHIPMENT: routine
    SAMPLE
    STABILITY: at least 6 weeks @ 25 C

    TEMPERATURE-INJECTION: 185 to 200 C


    -DETECTOR: 250 C
    -COLUMN: 160 to 200 C

    BLANKS:

    CARRIER GAS:

    N2, 30 mL/min

    COLUMN:

    stainless steel, 1.2 m 6-mm OD; 50/80


    mesh Porapak Q or equivalent

    CALIBRATION:

    standard solutions of allyl chloride in


    benzene

    RANGE:

    0.05 to 1.5 mg per sample

    2 to 10 field blanks per set


    ACCURACY

    RANGE STUDIED:
    BIAS:

    1.8 to 7.2 mg/m [1] (100-L


    samples)
    6.4%

    OVERALL PRECISION ( ): 0.071 [1]

    ESTIMATED LOD: 0.01 mg per sample


    ACCURACY:

    16.6%

    PRECISION ( ):

    0.023 [1]

    APPLICABILITY: The working range is 0.16 to 3 ppm (0.5 to 10 mg/m) for a 100-L air sample. The method is applicable to
    short-term samples taken at 1 L/min. The upper limit of loading depends on the concentrations of allyl chloride and other
    substances in the air, including water vapor.
    INTERFERENCES: None identified.
    OTHER METHODS: This is Method S116 in a revised format [2].

    NIOSH Manual of Analytical Methods (NMAM), Fourth Edition

    ALLYL CHLORIDE: METHOD 1000, Issue 2, dated 15 August 1994 - Page 2 of 3

    REAGENTS:

    EQUIPMENT:

    1. Benzene, chromatographic quality.*


    2. Allyl chloride.
    3. Hexane.
    4. Calibration stock solution, 7.5 g/L. Dilute 75
    mg allyl chloride (80.0 L at 20 C) to 10 mL
    with hexane.
    5. Nitrogen, purified.
    6. Hydrogen, prepurified.
    7. Air.
    *See SPECIAL PRECAUTIONS.

    1. Sampler: glass tube, 7 cm long, 6-mm OD,


    4-mm ID, flame-sealed ends, containing two
    sections of activated (600 C) coconut shell
    charcoal (front = 100 mg, back = 50 mg)
    separated by a 2-mm urethane foam plug. A
    silylated glass wool plug precedes the front
    section and a 3-mm urethane foam plug
    follows the back section. Pressure drop across
    the tube at 1 L/min airflow must be less than
    3.4 kPa. Tubes are commercially available.
    2. Personal sampling pump, 0.01 to 1 L/min, with
    flexible connecting tubing.
    3. Gas chromatograph, flame ionization detector,
    integrator, and column (page 1000-1).
    4. Vials, 2-mL, PTFE-lined caps.
    5. Syringe, 10-L, readable to 0.1 L.
    6. Volumetric flasks, 10-mL.

    SPECIAL PRECAUTIONS: Benzene is a suspected human carcinogen. All work should be performed in
    a hood.
    SAMPLING:
    1. Calibrate each personal sampling pump with a representative sampler in line.
    2. Break the ends of the sampler immediately before sampling. Attach sampler to personal sampling
    pump with flexible tubing.
    3. Sample at an accurately known flow rate between 0.01 and 1 L/min for a total sample size of 16 to
    100 L.
    4. Cap the samplers with plastic (not rubber) caps and pack securely for shipment.
    SAMPLE PREPARATION:
    5. Place the front and back sorbent sections of the sampler tube in separate vials. Discard the glass
    wool and foam plugs.
    6. Add 1.0 mL benzene to each vial. Attach crimp cap to each vial.
    7. Allow to stand 30 min with occasional agitation.
    CALIBRATION AND QUALITY CONTROL:
    8. Calibrate daily with at least six working standards over the range 0.01 to 1.5 mg allyl chloride per
    sample.
    a. Add known amounts of calibration stock solution to benzene in 10-mL volumetric flasks and
    dilute to the mark.
    b. Analyze together with samples and blanks (steps 11 and 12).
    c. Prepare calibration graph (peak area vs. mg allyl chloride).
    9. Determine desorption efficiency (DE) at least once for each batch of charcoal used for sampling in
    the calibration range (step 8). Prepare three tubes at each of five levels plus three media blanks.
    a. Remove and discard back sorbent section of a media blank sampler.
    b. Inject a known amount of calibration stock solution directly onto front sorbent section with a
    microliter syringe.
    NIOSH Manual of Analytical Methods (NMAM), Fourth Edition

    ALLYL CHLORIDE: METHOD 1000, Issue 2, dated 15 August 1994 - Page 3 of 3

    c. Cap the tube. Allow to stand overnight.


    d. Desorb (steps 5 through 7) and analyze together with working standards (steps 11 and 12).
    e. Prepare a graph of DE vs. mg allyl chloride recovered.
    10. Analyze three quality control blind spikes and three analyst spikes to insure that the calibration
    graph and DE graph are in control.
    MEASUREMENT:
    11. Set gas chromatograph according to manufacturers recommendations and to conditions given on
    page 1000-1. Inject sample aliquot manually using solvent flush technique or with autosampler.
    NOTE: If peak area is above the linear range of the working standards, dilute with benzene, reanalyze
    and apply the appropriate dilution factor in calculations.
    12. Measure peak area.
    CALCULATIONS:
    13. Determine the mass, mg (corrected for DE) of allyl chloride found in the sample front ( ) and back
    ( ) sorbent sections, and in the average media blank front ( ) and back ( ) sorbent sections.
    NOTE: If > /10, report breakthrough and possible sample loss.
    14. Calculate concentration, , of allyl chloride in the air volume sampled, (L):
    , mg/m.
    EVALUATION OF METHOD:
    Method S116 was issued on May 9, 1975 [2], and validated over the range 1.8 to 7.2 mg/m at 25 C and
    759 mm Hg using a 100-L sample [1]. Overall precision, , was 0.071 with average recovery 105.5%,
    representing a nonsignificant bias. The concentration of allyl chloride was independently verified
    by direct gas chromatography. Desorption efficiency was 0.943 in the range 0.15 mg to 0.6 mg allyl
    chloride per sample. Breakthrough (5% on back section) occurred between 210 and 240 min when
    sampling an atmosphere containing 7.56 mg/m allyl chloride at 0.94 L/min at 0% RH.
    REFERENCES:
    [1] Documentation of the NIOSH Validation Tests, NIOSH, S116, U.S. Department of Health, Education,
    and Welfare, Publ. (NIOSH) 77-185 (1977).
    [2] NIOSH Manual of Analytical Methods, 2nd ed., V. 2, S116, U.S. Department of Health, Education, and
    Welfare, Publ. (NIOSH) 77-157-B (1977).
    METHOD REVISED BY:
    G. David Foley, NIOSH/DPSE; originally validated under NIOSH Contract CDC-99-74-45.

    NIOSH Manual of Analytical Methods (NMAM), Fourth Edition

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