Semi Volatiles - Derivatised

Volatiles

Basis of Test / Purge & Trap or Headspace GCMS, full scan EI mode (e.g. EPA 8260)
Mass Scan Range / 35 to 300
Lower Reporting Level for core determinands / <10 µg/l
Core Determinands (C.D.) / chlorobenzene, trichloroethene, tetrachloroethene, 1,2 dichlorobenzene
Precision % (on C.D.) / 25 @ 100 µg/l
Bias % (on C.D.) / 20
Spiking Recovery % (on C.D.) / >50
Internal Standards (I.S.) / eg pentafluorobenzene, difluorobenzene, chlorobenzene-d5, 1,4-dichlorobenzene-d4 (required to overlap with semi-volatile analysis). Surrogates e.g. BCTFE, fluorobenzene, p-bromofluorobenzene (BFB), dibromofluorometane, toluene-d8. Use a minimum of 3 surrogates.
Calibration / Normal MS tune/sensitivity checks. Calibrate using C.D./I.S.
Minimum QC requirements / 1 AQC sample (C.D. @ ~ 100 µg/l plus I.S.) with every 10 samples, taken throughout the entire procedure
Reporting / Report all peaks with a library match confidence of >80%
Libraries / NIST, Wiley

Semi volatiles

Basis of Test / Liquid/liquid extraction (e.g. DCM, iso-hexane, hexane) at pH ~7 and pH>11, followed by GCMS full scan E1 mode
Mass Scan Range / 35 to 650
Lower Reporting Level for core determinands / <10 µg/l
Core Determinands (C.D.) / Aldrin, pentachlorobenzene, malathion, trifluralin, atrazine
Precision % (on C.D.) / 25 @ 100 µg/l
Bias % (on C.D.) / 20
Spiking Recovery % (on C.D.) / >50
Internal Standards (I.S.) / eg 1,4-dichlorobenzene-d4 (required to overlap with semi-volatile analysis), naphthalene-d8, phenanthrened10, perylene-d12. Surrogates e.g. decafluorobiphenyl, 4- fluoroaniline, 2-fluoronaphthalene. Use a minimum of 3 surrogates
Calibration / Normal MS tune/sensitivity checks. Calibrate using C.D./I.S.
Minimum QC requirements / 1 AQC sample (C.D. @ ~ 100 µg/l plus I.S.) with every 10 samples, taken throughout the entire procedure
Reporting / Report all peaks with a library match confidence of >80%
Libraries / NIST, Wiley

Semi volatiles - derivatised

Basis of Test / Liquid/liquid extraction (e.g. DCM, iso-hexane, hexane) at pH
Mass Scan Range / 35 to 650
Lower Reporting Level for core determinands / <10 µg/l
Core Determinands (C.D.) / 2-chlorophenol, dichlorprop, PCP, bromoxynil, 2,4,6-trichlorophenol, ioxynil
Precision % (on C.D.) / 25 @ 100 µg/l
Bias % (on C.D.) / 20
Spiking Recovery % (on C.D.) / <50
Internal Standards (I.S.) / 1,4-dichlorobenzene-d4, naphthalene-d8, phenanthrene-d10, chrysene-d12, perylene-d12. Surrogates e.g. 2,3,5,6- tetrafluorobenzoic acid, 1,2,3-trichloropropane, 4,4-dibromooctafluorobiphenyl, 2,4,5,6-tetrachloro-m-xylene. Use a minimum of 2 surrogates
Calibration / Normal MS tune/sensitivity checks. Calibrate using C.D./I.S.
Minimum QC requirements / 1 AQC sample (C.D. @ ~ 100 µg/l plus I.S.) with every 10 samples, taken throughout the entire procedure
Reporting / Report all peaks with a library match confidence of >80%
Libraries / NIST, Wiley

# Laboratories using diazomethane should be aware of the extreme health and safety hazards associated with this reagent, and have effective risk-management measures in place. Tetramethyl anilinium hydroxide (TMAH) has proved to be an effective alternative methylating agent with less significant heath and safety hazards, which are more easily controlled.

Organotin compounds

Basis of Test / Liquid/liquid extraction (e.g. toluene, hexane/tropolone etc.) followed by EAAS (e.g. SCA 1992 method, ISBN 9 780117 523609) or GC-MS/FPD/AED
Lower Reporting Level / <1 µg/l
Core Determinands (C.D.) / bis(tributyltin) oxide or tributyltin chloride, triphenyltin chloride
Precision % (on C.D.) / 10 @ 10 µg/l or 25 @ 0.1 μg/l
Bias % (on C.D.) / 10
Spiking Recovery % (on C.D.) / >85
Calibration / Normal instrument tune/sensitivity checks. Calibrate using C.D. standard with I.S. standard when undertaking GC procedures.
Minimum QC requirements / 1 AQC sample (C.D. @ ~ 10 µg/l, or lower for GC procedure, e.g. 0.1μg/l) with every 10 samples, taken throughout the entire procedure.
Reporting / Report as total organotin (EAAS) or as individual compounds for GC procedure.

Mercury

Basis of Test / Mercury compounds reduced to elemental mercury (eg using stannous chloride) then measured by AFS or Cold Vapour AAS
Lower Reporting Level / <1 µg/l
Core Determinands (C.D.) / Mercury (II) nitrate
Precision % (on C.D.) / 10 @ 10 µg/l
Bias % (on C.D.) / 10
Spiking Recovery % (on C.D.) / >75
Calibration / Normal instrument tune/sensitivity checks. Calibrate using C.D.
Minimum QC requirements / 1 AQC sample (C.D. @ ~ 10 µg/l) with every 10 samples, plus spiking recovery for each sample
Reporting / Report as total mercury.

Cadmium

Basis of Test / Cadmium compounds are brought into solution by acid digestion (e.g. HNO3) then measured by ICP or EAAS
Lower Reporting Level / <1 µg/l
Core Determinands (C.D.) / Cadmium Chloride
Precision % (on C.D.) / 10 @ 10 µg/l
Bias % (on C.D.) / 10
Spiking Recovery % (on C.D.) / >75
Calibration / Normal instrument tune/sensitivity checks. Calibrate using C.D.
Minimum QC requirements / 1 AQC sample (C.D. @ ~ 10 µg/l) with every 10 samples, plus spiking recovery for each sample matrix
Reporting / Report as total cadmium.