Poisoned food sample (10-30 g) was ground with some anhydrous Na₂SO₄ and the mixture was agitated with 70 ml CH₂Cl₂ for 30 min. After filtration, the filtrate was evaporated to dryness and the residue was dissolved in and diluted with acetone to 10 ml. Portions (2 l) were analysed for two rat toxicants and five organophosphorus pesticides (viz. fluoroacetamide, phosazetim, DDVP, methamidophos, dimethoate, malathion and parathion) by GC on a fused-silica column (30 m �0.25 mm i.d.) coated with HP-5MS (0.25m), operated with temperature programming from 50�C (held for 3 min) to 130�C (held for 3 min) at 20�C/min, and finally to 190�C (held for 10 min) at 30�C/min and EIMS detection. Results are discussed.

With Chromosorb 106 (I), Tenax TA and Tenax TG as adsorbents, the breakthrough volumes of 23 VOCs (mainly alcohols, esters, ketones, alkanes, alkenes and haloalkanes) were determined in which four mixtures of VOC with N₂ carrier gas were allowed to pass through the sorbent-packed tubes prior to thermal desorption and GC-MS analysis. Results indicated that I was a better sorbent for low-boiling VOC than the others, with a breakthrough volume of <2 l at flow-rate of 100 ml/min except methanol, and there was no significant difference in performance between the other two for adsorbing high-boiling compounds. These sorbents are applicable in sampling e.g. air.

A review is presented of developments in the analysis of SO₂ in food and the environment, with particular emphasis on techniques like spectrophotometry, electrochemical methods and sensors, chromatography and chemiluminescence. (44 references).

Sulfur dioxide (I)-containing air was sampled for 2 h at 1 l/min into 10 ml aqueous 0.1% triethanolamine as absorption solution. Portions of the solution were heated with 0.2 ml 40 g/ml tris(1,10-phenanthroline)ruthenium(II) dibromide and 0.2 ml 0.5mM-sodium dodecylbenzenesulfonate at 25�C for 5 min. A 0.2 ml portion of 1M-K₂S₂O₈ containing 0.05M-H₂SO₄ was added and the chemiluminescence intensity was measured. The amount of sulfite was calculated from the calibration graph which was linear from 175nM to 125M-I with a detection limit of 6nM. The recoveries of 6-10M-I from clean air were 92.6-99.8%. No interference was observed.

A review of the advances in chemiluminescence (CL) analysis over the past three years is presented. New CL reagents and applications in the analysis of inorganic and organic compounds, pharmaceuticals and biologically-active substances, as well as some hyphenated techniques are discussed in detail. (113 references).

HPLC was performed using a 5 m C₁₈ reverse phase column (15 cm �4.6 mm i.d.) with 0.02M-ammonium acetate as mobile phase. The eluate was mixed with 0.25mM-tris(1,10-phenanthroline)ruthenium(II) which then flowed into the chamber of a luminometer where it was mixed with a stream of 2mM-Ce(IV) sulfate in 0.08mM-H₂SO₄. The light emitted was detected. The detection limit was 6.2M-oxalic acid at a signal:noise ratio of 3, the RSD (n = 5) for 1mM-oxalic acid was 5.6% and the calibration graph was linear from 10M to 4mM. The method was applied to the determination of oxalic acid in spinach after drying, powdering, boiling in aqueous solution and filtering (details given).

Thiourea (I, 0.2 ml), was mixed sequentially with 0.2 ml 2mM-sodium dodecyl benzene sulfonate and 0.2 ml of 22.4 g/ml of tris(2,2'-bipyridyl)ruthenium(II). The mixture was transferred to the measuring chamber of a LKB 1251 luminometer (Pharmacia LKB Biotechnology AB, Sweden) where 0.2 ml 0.1mM-KMnO₄ (in 0.03M-H₂SO₄) was injected automatically and the peak height of the emission intensity was measured vs. a reagent blank prepared similarly using H₂O instead of I. Commonly used ions and solvents did not interfere. The calibration graph was linear from 18nM to 1.8M with a detection limit of 10nM. The RSD (n = 10) was 1.1% at the 11M level. The method was applied to the determination of I in white wine.

Sugar was dissolved in H₂O. Air was passed (1 l/min) through 0.1% triethanolamine (TEA) for 2 h. For sulfite/SO₂ determination, a portion (0.2 ml) of the sample solution was mixed with 0.2 ml of 44.8 g/ml tris(2,2'-bipyridyl)ruthenium(II) and 0.2 ml 2mM-sodium dodecyl benzenesulfonate. Then, 0.2 ml 50M-KMnO₄ in 10mM-H₂SO₄ was added and the chemiluminescence intensity was recorded. The calibration graph was linear for 0.05-125M-sulfite (0.1-12.5M-sulfite in TEA), the detection limit was 25nM, the RSD (n = 6) at the 20M-sulfite level was 4.9% and the recoveries were 90-105%.

Triethanolamine (10 ml of 0.05%) was added to the air sampling flasks and air was pumped through the flask for 2 h at 1 ml/min. For the analysis an LKB 1251 Luminometer was used. A 0.2 ml portion of 20 g/ml Ru(1,10-phenanthroline)₃Br²⁺, 0.2 ml 0.5mM-sodium dodecyl benzene sulfonate and 0.2 ml triethanolamine extract were transferred into the measuring chamber at 25��C. After starting the instrument 0.2 ml 0.2mM-KIO₄ in 50mM-sulfuric acid was injected automatically and the peak height recorded. Calibration graphs of emission intensity vs. sulfite concentration were linear over the range 0.1M to 0.15mM. The detection limit was 0.7nM and the RSD (n = 9) at 40M was 2.3%.

The title reagent was used to enhance the chemiluminescent reaction between SO₃^2- and KMnO₄. Triethanolamine was used as absorbent to collect SO₂ from air. The calibration graph was linear for 1 �10^-7 to 2.5 � 10^-5 mol/l SO₃^2-. The detection limit was 4.5 �10^-9 and the RSD (n=8) was 3.1% for 1 � 10^-5 SO₃^2-.

Tris(2,2'-bipyridyl)ruthenium (0.2 ml, 44.8 g/ml), 0.2 ml 0.8mM-sodium dodecyl benzene sulfonate and 0.2 ml aqueous sample solution (or calibration solution containing from 1-50M-Na₂SO₃) were mixed in that order and then transferred to the luminometer chamber where 0.2 ml 0.2mM-KIO₄ was automatically added. The chemiluminescence was then measured. The sulfite concentration was proportional to the chemiluminescence intensity from 0.1M to 0.1mM with a detection limit of 20nM and an RSD of 4.4% for a 20M-sulfite solution. Air samples were prepared by passing air through 10 ml 0.1% aqueous triethanolamine to absorb the SO₂.

A 0.2 ml portion of 44.8M-Ru(bpy)₃²⁺ (bpy = 2,2'-bipyridyl) was mixed sequentially with 0.2 ml 0.86mM-sodium dodecylbenzenesulfonate and 0.2 ml of sulfite (I) standard solution. An 0.2 ml portion of 5.64mM-KBrO₃ in 20mM-H₂SO₄ was added and the chemiluminescence intensity was measured. The calibration graph was linear for 0.025-95M-I with a detection limit of 3.8nM. The RSD (n = 9) was 4.6% for 50M-I. The method was applied to the analysis of I in sugar solutions and SO₂ in air after collection of the SO₂ in 0.1% triethanolamine. The recoveries were 93-110%.

Ground tea (0.6 g) and 200 ml boiling water were transferred to a 250 ml flask, and the pH adjusted to 1-2 with 2M-HCl. After 30 min, the mixture was boiled further for 90 min and then cooled. The solution was filtered and diluted to 250 ml. Spiked samples were prepared by the addition of 0.5 or 1.0 ml 0.1M-oxalic acid (I. Analysis was performed on a 5 m C18 reversed-phase column (15 cm �4.6 mm i.d.), 20mM-ammonium acetate as mobile phase (1 ml/min), 0.25M-tris(1,10-phenanthroline)-ruthenium(II) and 2mM-cerium sulfate (0.7 ml/min) as post-column reagents, chemiluminescence detection. The calibration graph was linear from 10M to 0.4mM-I. The detection limit was 6.2M and the RSD (n = 5) was 5.6% for 1mM-I.

Solution of Ru(2,2'-bipyridyl)₃²⁺, sodium dodecylbenzene sulfonate and Na₂SO₃ were mixed. After the addition of K₂S₂O₈ in 0.05M-H₂SO₄, the intensity of the chemiluminescence was measured. The Na₂SO₃ concentration was found from a calibration graph. The method was used for the determination of sulfite in sugar or SO₂ in air after sorption in triethanolamine.

Sample (5 ml) was neutralized with aq. NH3 and filtered. A portion of the filtrate was analysed by HPLC on a column (10 cm �8 mm) of Bondapak C18 (10 m) with gradient elution (2 ml min-1) with 20mM-ammonium acetate - aq. methanol (details given) and detection at 230 nm. Detection limits for benzoic acid, saccharin, tartrazine (C. I. Food Yellow), amaranth (C. I. Food Red 9), ponceau 4R (C. I. Food Red 7), sunset yellow FCF (C. I. Food Yellow 3), caffeine and brilliant blue FCF (C. I. Food Blue 2) were 20, 5, 30, 17, 10, 15, 10, 15 and 35 ng, respectively. Recoveries ranged from 92 to 108% with coeff. of variation of 0.4 to 4.0%.

A portion (0.5 l) of a soln. (50 mg l-1) of crude acetofenate (I) in light petroleum is analysed by GC on a glass column (2.1 m �3.2 mm) of 2% of QF-1 on Chromosorb W-AW DMCS (80 to 100 mesh) operated at 180�� with N as carrier gas (50 ml min-1) and FID. The chromatogram of I is presented; two major impurities in I are separated. These compounds are not isomers of DDT because, under the same conditions, pp'-DDT, pp'-DDE, op'-DDT and TDE) can also be determined, and their peaks are not affected by the impurity peaks of I.