CN103364238A - Selective separation of PCNs (polychlorinated naphthalenes congeners), HBCDss (hexabromocyclododecanes) and TBBPA (tetrabromobisphenol A) in complex samples - Google Patents
Selective separation of PCNs (polychlorinated naphthalenes congeners), HBCDss (hexabromocyclododecanes) and TBBPA (tetrabromobisphenol A) in complex samples Download PDFInfo
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- CN103364238A CN103364238A CN2012101039137A CN201210103913A CN103364238A CN 103364238 A CN103364238 A CN 103364238A CN 2012101039137 A CN2012101039137 A CN 2012101039137A CN 201210103913 A CN201210103913 A CN 201210103913A CN 103364238 A CN103364238 A CN 103364238A
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- VEORPZCZECFIRK-UHFFFAOYSA-N 3,3',5,5'-tetrabromobisphenol A Chemical compound C=1C(Br)=C(O)C(Br)=CC=1C(C)(C)C1=CC(Br)=C(O)C(Br)=C1 VEORPZCZECFIRK-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 238000000926 separation method Methods 0.000 title claims abstract description 29
- 239000013260 porous coordination network Substances 0.000 title claims abstract description 6
- SHRRVNVEOIKVSG-UHFFFAOYSA-N 1,1,2,2,3,3-hexabromocyclododecane Chemical class BrC1(Br)CCCCCCCCCC(Br)(Br)C1(Br)Br SHRRVNVEOIKVSG-UHFFFAOYSA-N 0.000 title abstract 4
- 239000000039 congener Substances 0.000 title abstract 4
- 150000002790 naphthalenes Chemical class 0.000 title abstract 4
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims abstract description 90
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 52
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000000945 filler Substances 0.000 claims abstract description 19
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 17
- 239000002904 solvent Substances 0.000 claims abstract description 17
- 239000011159 matrix material Substances 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000003960 organic solvent Substances 0.000 claims abstract description 9
- 238000000638 solvent extraction Methods 0.000 claims abstract description 4
- DEIGXXQKDWULML-UHFFFAOYSA-N 1,2,5,6,9,10-hexabromocyclododecane Chemical compound BrC1CCC(Br)C(Br)CCC(Br)C(Br)CCC1Br DEIGXXQKDWULML-UHFFFAOYSA-N 0.000 claims description 35
- JTPNRXUCIXHOKM-UHFFFAOYSA-N 1-chloronaphthalene Chemical class C1=CC=C2C(Cl)=CC=CC2=C1 JTPNRXUCIXHOKM-UHFFFAOYSA-N 0.000 claims description 27
- 239000000523 sample Substances 0.000 claims description 19
- 239000012046 mixed solvent Substances 0.000 claims description 18
- 239000000741 silica gel Substances 0.000 claims description 17
- 229910002027 silica gel Inorganic materials 0.000 claims description 17
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 12
- 239000003480 eluent Substances 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- 239000002689 soil Substances 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 239000012472 biological sample Substances 0.000 claims description 3
- 230000009849 deactivation Effects 0.000 claims description 3
- 238000002414 normal-phase solid-phase extraction Methods 0.000 claims description 3
- 239000013049 sediment Substances 0.000 claims description 3
- 230000004913 activation Effects 0.000 claims description 2
- 239000003463 adsorbent Substances 0.000 claims 1
- 230000008901 benefit Effects 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 3
- 238000001819 mass spectrum Methods 0.000 description 7
- 239000003344 environmental pollutant Substances 0.000 description 6
- 231100000719 pollutant Toxicity 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 4
- 238000002390 rotary evaporation Methods 0.000 description 4
- 239000000356 contaminant Substances 0.000 description 3
- 238000004817 gas chromatography Methods 0.000 description 3
- 238000004128 high performance liquid chromatography Methods 0.000 description 3
- 230000035945 sensitivity Effects 0.000 description 3
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical class N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 2
- 238000000944 Soxhlet extraction Methods 0.000 description 2
- 239000012491 analyte Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 230000002688 persistence Effects 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 238000012113 quantitative test Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000013459 approach Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- ZCILODAAHLISPY-UHFFFAOYSA-N biphenyl ether Natural products C1=C(CC=C)C(O)=CC(OC=2C(=CC(CC=C)=CC=2)O)=C1 ZCILODAAHLISPY-UHFFFAOYSA-N 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 150000003071 polychlorinated biphenyls Chemical group 0.000 description 1
- 229920006327 polystyrene foam Polymers 0.000 description 1
- 238000000899 pressurised-fluid extraction Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000002000 scavenging effect Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- FKHIFSZMMVMEQY-UHFFFAOYSA-N talc Chemical compound [Mg+2].[O-][Si]([O-])=O FKHIFSZMMVMEQY-UHFFFAOYSA-N 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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Abstract
The invention relates to utilization of a silica matrix as a sample pretreatment material, wherein a) PCNs (polychlorinated naphthalenes congeners), HBCDs (hexabromocyclododecanes) and TBBPA (tetrabromobisphenol A) in complex samples are extracted by a solvent extraction method and an extract containing target analytes is obtained; b) the silica matrix is selected as a chromatographic column filler; the filer is activated by using normal hexane at first and then the extract is loaded; c) the polychlorinated naphthalenes congeners, hexabromocyclododecanes and tetrabromobisphenol A are eluted orderly by using organic solvents (normal hexane, dichloromethane and the like) composed of different solvents, and then three eluates of different fractions are obtained; d) after solvents are volatilized from the eluates, the purified target analytes are obtained. According to the invention, selective separation of the polychlorinated naphthalenes congeners, hexabromocyclododecanes and tetrabromobisphenol A in the complex samples is realized by virtue of a simple chromatographic column; the method has the advantages of simplicity in operation, good selectivity and high efficiency.
Description
Technical field
The present invention relates to the selective separation method of many chloronaphthalenes (PCNs) in the complex sample, hexabromo-Cyclododecane (HBCDs) and tetrabromobisphenol A (TBBPA), specifically a kind of silica matrix that utilizes carries out three class materials in sediment, soil and the biological sample method of Selective Separation as the chromatographic column filler.
Background technology
The commercialization hexabromo-Cyclododecane is commonly used in the polystyrene foam, because its output is high, has again the feature of persistence organic pollutant simultaneously, is defined as priority pollutants and high yield chemicals by European chemicals management board.Tetrabromobisphenol A is a kind of response type brominated flame-retardant, is commonly used in the circuit board, is the flame retardant products of present use amount maximum.As one of ubiquitous organic contaminant, in a lot of surrounding mediums, be detected.Many chloronaphthalenes can carry out long-distance transmissions by atmosphere, united state Economic Commission for Europe, world's conservation of wildlife foundation recommend to list in " about and the Convention of Stockholm of organic contaminant just " preferentially control in the waiting list of persistence organic pollutant.At present, the environmental pollution that causes of this three pollutant has become a large focus of Research of Environmental Sciences.
Consider the difference of three pollutant character, can carry out quantitative test to PCNs by the gas chromatography-mass spectrum technology, and by the quantitative test of liquid chromatography-mass spectrography realization to hexabromo-Cyclododecane and tetrabromobisphenol A.Therefore in sample pretreatment process, many chloronaphthalenes and other two kinds of separated from contaminants must be opened.Simultaneously, because hexabromo-Cyclododecane is than the difficult ionization of tetrabromobisphenol A, so in the analytical test process, its degree of ionization is little, a little less than the response signal, have a strong impact on the sensitivity of analytical test and property again.So hexabromo-Cyclododecane and tetrabromobisphenol A are separated by pretreatment technology, for the content of measuring more accurately hexabromo-Cyclododecane, the sensitivity tool that improves analytical approach is of great significance.At present, studies show that, silica matrix, florisil silica all can be used as scavenging material, by changing the polarity of organic solvent in the purification process, realize (the U.Berger that separates of hexabromo-Cyclododecane, tetrabromobisphenol A and polychlorinated biphenyl ether, D.Herzke, T.M.Sandanger, Anal.Chem.76 (2004) 441-452; S.Morris, C.R.Allchin, B.N.Zegers, J.J.H.Haftka, J.P.Boon, C.Belpaire, P.E.G.Leonards, S.P.J.Van Leeuwen, J.De Boer, Environ.Sci.Technol.38 (2004) 5497-5504).In addition, 0asis HLB solid-phase extraction column also is used to separate fast hexabromo-Cyclododecane and tetrabromobisphenol A (R.Cariou, J.P.Antignac, P.Marchand, A.Berrebi, D.Zalko, F.Andre, B.Le Bizec, J.Chromatogr.A 1100 (2005) 144-152).Consider that HLB solid-phase extraction column cost is higher, generally still adopt chromatographic column to realize the separation of pollutant.Yet, about the Selective Separation of many chloronaphthalenes, hexabromo-Cyclododecane and tetrabromobisphenol A report had not been arranged also.Set up the selective separation method of tertiary target analyte, effectively monitor for realization heterogeneity analyte, improve sensitivity and the accuracy analyzed and have great importance.
Summary of the invention
The object of the invention is to develop a kind of simple to operate, selectivity good, separation efficiency is high selective separation method, be used for realizing separating of many chloronaphthalenes, hexabromo-Cyclododecane and tetrabromobisphenol A.
For solving the problems of the technologies described above, the technical solution adopted in the present invention is:
The selective separation method of many chloronaphthalenes, hexabromo-Cyclododecane and tetrabromobisphenol A in a kind of complex sample utilizes silica matrix to be used for optionally three kinds of pollutants of separate complex sample as the chromatographic column filler, and its operation steps is as follows:
A) adopt solvent extraction that many chloronaphthalenes, hexabromo-Cyclododecane and tetrabromobisphenol A in the complex sample are extracted, must contain the extract of target analytes; The solvent that adopts is the mixed solvent of normal hexane, methylene chloride; The volume ratio of normal hexane and methylene chloride is 2 in the mixed solvent: 1-1: 9;
B) silica matrix is closely packed in the chromatographic column, after normal hexane to be used carries out the drip washing activation, will contain the extract loading of target analytes;
C) adopting successively normal hexane, volume ratio is 1: the mixed solvent of 1-3 normal hexane and methylene chloride, the dichloromethane solvent that contains volumetric concentration 0-3% acetic acid carry out wash-out, carry out respectively fraction collection by three kinds of different eluents, get three kinds of different fractions;
D) three kinds of different fractions are respectively behind the solvent flashing, namely obtain through Selective Separation, be in the many chloronaphthalenes of target compound, hexabromo-Cyclododecane and the tetrabromobisphenol A in the different fractions one or more.
Described solvent extraction is soxhlet extraction or accelerated solvent extraction;
Complex sample is 2-10g: 200-300mL with the solvent load ratio among the step a;
The mass ratio 3-8 of silica matrix consumption and complex sample: 2-10 among the step b, employed silica matrix can be commercial silica gel, also can be the silica gel that adopts after deionized water carries out partly deactivating to it, the deionized water that adds and the mass ratio of silica gel be 1-5: 100.
The kind of employed organic solvent is relevant with the kind of silica matrix with consumption among the step c.When take commercialization silica gel as the chromatographic column filler, the solvent that adopts of the many chloronaphthalenes of wash-out, hexabromo-Cyclododecane and tetrabromobisphenol A is respectively that (volume ratio is 1: 1-3), and the methylene chloride that adds 0.1-3% (volume ratio) acetic acid for the mixed solution of normal hexane, normal hexane and methylene chloride successively.Wherein chromatographic column filler and consumption of organic solvent are than being 3-8g: 150-300mL.When take the silica gel that deactivates of part during as the chromatographic column filler, the solvent that adopts of the above-mentioned three kinds of organism of wash-out is respectively normal hexane, normal hexane and methylene chloride mixed solvent (volume ratio 1: 0.5-1), and normal hexane and methylene chloride mixed solvent (volume ratio 1: 3-10) successively.Chromatographic column filler and consumption of organic solvent are than being 3-8g: 100-200mL.
Described complex sample refers to soil, river or Marine Sediment, biological sample.
The present invention has following advantage:
(1) simple to operate: as can to realize Selective Separation (2) the method selectivity good separating effect to many chloronaphthalenes, hexabromo-Cyclododecane and tetrabromobisphenol A in the complex sample substantially not having intersection (3) separation efficiency of target analytes between different fractions high by simple chromatography process once.
It is the chromatographic column filler that the present invention adopts the silica matrix that easily obtains on the market, by the adjustment to its activity, selects the suitable organic solvent of polarity, has realized the Selective Separation to many chloronaphthalenes, hexabromo-Cyclododecane and tetrabromobisphenol A in the complex sample.
Description of drawings
Fig. 1 take silica matrix as the chromatographic column filler, has realized the Selective Separation to many chloronaphthalenes, hexabromo-Cyclododecane and tetrabromobisphenol A for adopting the inventive method.
Fig. 2 take the part deactivated silica gel as the chromatographic column filler, has realized the Selective Separation to many chloronaphthalenes, hexabromo-Cyclododecane and tetrabromobisphenol A for adopting the inventive method.
Embodiment
Embodiment 1:
8g silica gel is closely packed in the chromatographic column (external diameter 26mm, length 305mm), and use vacuum pump that this filler is taken out reality.Before the loading, use the 50mL normal hexane that chromatographic column is activated; Then with mixed mark (many chloronaphthalenes 100ng mL of the many chloronaphthalenes of 1mL, hexabromo-Cyclododecane and tetrabromobisphenol A
-1, hexabromo-Cyclododecane 500ng mL
-1, tetrabromobisphenol A 500ng mL
-1, surplus is the normal hexane solvent) and loading.Loading is complete, uses successively 200mL normal hexane, 200mL normal hexane and methylene chloride mixed solvent (volume ratio 1: 1), and 4 * 50mL methylene chloride carries out wash-out, obtains six groups of different eluents.With constant volume behind six groups of eluent rotary evaporations, carry out again gas chromatography tandem mass spectrum or using high performance liquid chromatography tandem mass spectrum analysis.
As can be seen from Figure 1, when take silica gel as the chromatographic column filler, the 200mL normal hexane can elute many chloronaphthalenes, does not disturb the mensuration of hexabromo-Cyclododecane and tetrabromobisphenol A; And the 200mL volume ratio to be 1: 1 normal hexane and the mixed solvent of methylene chloride can elute hexabromo-Cyclododecane, realize separating of hexabromo-Cyclododecane and tetrabromobisphenol A.
Embodiment 2:
In the silica gel that 8g 3% is deactivated (adopting deionized water and the mass ratio of silica gel is to mix at 3: 100, the carries out deactivation process) chromatographic column of closely packing into (external diameter 26mm, length 305mm), and the use vacuum pump is taken out reality with this filler.Before the loading, use the 50mL normal hexane that chromatographic column is activated; Then with mixed mark (many chloronaphthalenes 100ng mL of the many chloronaphthalenes of 1mL, hexabromo-Cyclododecane and tetrabromobisphenol A
-1, hexabromo-Cyclododecane 500ng mL
-1, tetrabromobisphenol A 500ng mL
-1, surplus is the normal hexane solvent) and loading.Loading is complete, use successively 100mL normal hexane, 2 * 50mL normal hexane and methylene chloride mixed solvent (volume ratio 1: 1), 2 * 50mL normal hexane and methylene chloride mixed solvent (volume ratio 1: 3) and 2 * 50mL methylene chloride carry out wash-out, obtain seven groups of different eluents.With constant volume behind seven groups of eluent rotary evaporations, carry out again gas chromatography tandem mass spectrum or using high performance liquid chromatography tandem mass spectrum analysis.
As can be seen from Figure 2, with 3% silica gel that deactivates during as the chromatographic column filler, the 100mL normal hexane elutes many chloronaphthalenes from chromatographic column after, the 100mL volume ratio is that 1: 1 normal hexane and the mixed solvent of methylene chloride can elute hexabromo-Cyclododecane, do not disturb the reservation of tetrabromobisphenol A on chromatographic column, thereby realize the effective separation of the two.Three's separation efficiency is all more than 86%, and wherein hexabromo-Cyclododecane and tetrabromobisphenol A are realized complete wash-out substantially.
Embodiment 3:
Utilize first the soxhlet extraction method that 10g soil is extracted (extraction solvent is that the 250mL volume ratio is 1: 1 normal hexane and methylene chloride mixed solvent), by rotary evaporation the extract that contains target analytes is concentrated again, after being concentrated into about 500 μ L, use again normal hexane drip washing flat bottom flask three times, then leacheate is transferred in the test tube and constant volume to 10mL.
In the silica gel that 8g 3% is deactivated (adopting deionized water and the mass ratio of silica gel is to mix at 3: 100, the carries out deactivation process) chromatographic column of closely packing into (external diameter 26mm, length 305mm), and the use vacuum pump is taken out reality with this filler.Before the loading, use the 50mL normal hexane that chromatographic column is activated; Then 1mL has been added the mixed mark of many chloronaphthalenes, hexabromo-Cyclododecane and tetrabromobisphenol A (many chloronaphthalenes 100ngmL
-1, hexabromo-Cyclododecane 500ng mL
-1, tetrabromobisphenol A 500ng mL
-1) the extract loading.Loading is complete, uses successively 100mL normal hexane, 100mL normal hexane and methylene chloride mixed solvent (volume ratio 1: 1), and 100mL normal hexane and methylene chloride mixed solvent (volume ratio 1: 3) carry out wash-out, obtains three groups of different eluents.With constant volume behind three groups of eluent rotary evaporations, carry out again gas chromatography tandem mass spectrum or using high performance liquid chromatography tandem mass spectrum analysis.
Table 1 is to use selective separation method that pedotheque is processed rear resulting three kinds of pollutant recovery.Therefrom can find out, this selective separation method can be realized the effective separation to many chloronaphthalenes, hexabromo-Cyclododecane and tetrabromobisphenol A in the complex sample.
The recovery of the different drip washing step of table 1 gained target compound
Step 1, the 100mL normal hexane;
Step 2,100mL normal hexane and methylene chloride mixed solution (volume ratio 1: 1);
Step 3,100mL normal hexane and methylene chloride mixed solution (volume ratio 1: 3)
This invention has namely realized Selective Separation to many chloronaphthalenes, hexabromo-Cyclododecane and tetrabromobisphenol A in the complex sample by a simple chromatographic column, have advantages of simple to operate, selectivity good, efficient is high.
Claims (5)
1. the Selective Separation of PCNs, HBCDs and TBBPA in the complex sample is characterized in that:
Utilize silica matrix as solid phase extraction adsorbents, be used for one or more compounds that separate complex sample optionally comprises many chloronaphthalenes, hexabromo-Cyclododecane and tetrabromobisphenol A, its operation steps is as follows:
A) adopt solvent extraction that many chloronaphthalenes, hexabromo-Cyclododecane and tetrabromobisphenol A in the complex sample are extracted, must contain the extract of target analytes; The solvent that adopts is the mixed solvent of normal hexane, methylene chloride; The volume ratio of normal hexane and methylene chloride is 2 in the mixed solvent: 1-1: 9;
B) silica matrix is closely packed in the chromatographic column, after normal hexane to be used carries out the drip washing activation, will contain the extract loading of target analytes;
C) adopting successively normal hexane, volume ratio is 1: the mixed solvent of 1-3 normal hexane and methylene chloride, the dichloromethane solvent that contains volumetric concentration 0-3% acetic acid carry out wash-out, carry out respectively fraction collection by three kinds of different eluents, get three kinds of different fractions;
D) after three kinds of different fractions are distinguished solvent flashing, namely obtain through Selective Separation, be in the target compound in the different fractions, be i.e. one or more in many chloronaphthalenes, hexabromo-Cyclododecane and the tetrabromobisphenol A.
2. according to Selective Separation claimed in claim 1, it is characterized in that: complex sample is 2-10g: 200-300mL with the solvent load ratio among the step a;
The mass ratio 3-8 of silica matrix consumption and complex sample: 2-10 among the step b, employed silica matrix can be commercial silica gel, or adopting deionized water that it is carried out silica gel after part is deactivated, the deionized water that deactivation process is added and the mass ratio of silica gel are 1-5: 100;
The kind of employed organic solvent is relevant with the kind of silica matrix with consumption among the step c.
3. according to Selective Separation claimed in claim 2, it is characterized in that: among the step c when take commercialization silica gel as the chromatographic column filler, the solvent that adopts of the many chloronaphthalenes of wash-out, hexabromo-Cyclododecane and tetrabromobisphenol A is respectively that (volume ratio is 1: 1-3), and the methylene chloride that adds 0.1-3% (volume ratio) acetic acid for the mixed solution of normal hexane, normal hexane and methylene chloride successively; Wherein chromatographic column filler and consumption of organic solvent are than being 3-8g: 100-200mL.
4. according to Selective Separation claimed in claim 2, it is characterized in that: when take the silica gel that deactivates of part during as the chromatographic column filler, the solvent that adopts of the above-mentioned three kinds of organism of wash-out is respectively normal hexane, normal hexane and methylene chloride mixed solvent (volume ratio 1: 0.5-1), methylene chloride or normal hexane and methylene chloride mixed solvent (volume ratio 1: 3-10) successively among the step c; Wherein chromatographic column filler and consumption of organic solvent are than being 3-8g: 100-200mL.
5. according to Selective Separation claimed in claim 1, it is characterized in that: described complex sample refers to soil, river or Marine Sediment, biological sample.
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| CN113990407A (en) * | 2021-10-27 | 2022-01-28 | 北京中科三清环境技术有限公司 | Analytic method for analyzing content and source of polychlorinated naphthalene and homologues thereof |
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