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GB 17378.6-2007: The specification for marine monitoring -- Part 6: Organism analysis
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Basic data | Standard ID | GB 17378.6-2007 (GB17378.6-2007) | | Description (Translated English) | The specification for marine monitoring -- Part 6: Organism analysis | | Sector / Industry | National Standard | | Classification of Chinese Standard | A45 | | Classification of International Standard | 07.060 | | Word Count Estimation | 79,715 | | Date of Issue | 2007-10-18 | | Date of Implementation | 2008-05-01 | | Older Standard (superseded by this standard) | GB 17378.6-1998 | | Quoted Standard | GB 17378.3; GB 17378.4; GB 17378.5 | | Regulation (derived from) | Announcement of Newly Approved National Standards No. 12 of 2007 (total 112) | | Issuing agency(ies) | General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China, Standardization Administration of the People's Republic of China | | Summary | This Chinese standard provides mussels, shrimp, and fish and other marine organisms harmful residues Determination methods, and sample collection, transport, storage, pretreatment and determination of the calculation of the results proposed technical requirements. This standard applies to oceans, coastal waters, marine and coastal biological contamination investigation and monitoring. | GB 17378.6-2007: The specification for marine monitoring -- Part 6: Organism analysis---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
The specification for marine monitoring.Part 6. Organisim analysis
ICS 07.060
A45
National Standards of People's Republic of China
Replacing GB 17378.6-1998
Marine monitoring
Part 6. Analysis of the organism
Posted 2007-10-18
2008-05-01 implementation
Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China
Standardization Administration of China released
Table of Contents
Introduction Ⅲ
1 Scope 1
2 Normative references 1
3 Terms and definitions
4 1 General Provisions
5 5 Total Mercury
5 5.1 Atomic Fluorescence Spectrometry
5.2 Cold atomic absorption spectrophotometry 7
6 copper 9
6.1 flameless atomic absorption spectrophotometry (continuous determination of copper, lead and cadmium) 9
11 6.2 anodic stripping voltammetry
6.3 Flame Atomic Absorption Spectrometry 13
7 lead 14
7.1 flameless atomic absorption spectrophotometry 14
14 7.2 anodic stripping voltammetry
7.3 Flame Atomic Absorption Spectrometry 16
8 Cd 17
8.1 flameless atomic absorption spectrophotometry 17
17 8.2 anodic stripping voltammetry
8.3 Flame Atomic Absorption Spectrometry 19
9 Zinc 20
9.1 Flame Atomic Absorption Spectrometry 20
21 9.2 anodic stripping voltammetry
10 Cr 23
10.1 flameless atomic absorption spectrophotometry 23
10.2 diphenyl hydrazine spectrophotometry 24
Arsenic 11 26
11.1 Atomic Fluorescence Spectrometry 26
11.2 Arsenomolybdate - crystal violet spectrophotometric 28
11.3 hydride generation atomic absorption spectrophotometry 31
11.4 catalytic polarography 33
12 Selenium 35
12.1 fluorospectrophotometry 35
12.2 diaminobenzidine tetrahydrochloride salt spectrophotometric method 37
12.3 catalytic polarography 39
13 petroleum hydrocarbons --- fluorospectrophotometry 41
14 666, DDT --- Gas Chromatography 43
PCBs 15 47 --- Gas Chromatography
16 Dieldrin --- GC 49
Appendix A (normative) Table 50 records
Annex B (informative) Method Detection Limit 66
Annex C (informative) organochlorine pesticides --- Capillary Gas Chromatography 67
Annex D (informative) PCBs --- Capillary Gas Chromatography 71
Figure 1 cold vapor atomic absorption mercury device 8
Figure 2 column 45
Table 1 Analysis of samples taken from the sample to check the proportion of 5
Table 2 parallel double sample relative deviation Table 5
Table 3 content of each component of organochlorine pesticides in the list of 44 standard solution
Table A. 1 standard analysis of biological samples (work) curve data record (Atomic Fluorescence Spectrometry) 50
Table A. 2 biological sample analysis records (Atomic Fluorescence Spectrometry) 51
Table A. 3 standard analysis of biological samples (work) curve data record (spectrophotometry) 52
Table A. 4 biological sample analysis records (spectrophotometry) 53
Table A. 5 standard analysis of biological samples (work) curve data record (flameless atomic absorption spectrophotometry) 54
Table A. 6 biological sample analysis records (flameless atomic absorption spectrophotometry) 55
Table A. 7 biological sample analysis records (anodic stripping voltammetry) 56
Table A. 8 standard analysis of biological samples (work) curve data record (atomic absorption spectrophotometry) 57
Table A. 9 biological sample analysis records (atomic absorption spectrophotometry) 58
Table A. 10 biological sample standard (work) curve data record (Polarography) 59
Table A. 11 biological sample analysis records (Polarography) 60
Table A. 12 standard analysis of biological samples (work) curve data recording (fluorescence spectroscopy) 61
Table A. 13 biological sample analysis records (fluorescence spectroscopy) 62
Table A. 14 in a biological sample 666, DDT, dieldrin analysis records (GC) 63
Table A. 15 PCB biological sample analysis records (GC) 64
Table A. Monitoring of marine organisms 16 analysis reports 65
Table B. Determination of the detection limit of 66 1
Table C. 1 marine biological sample analysis of organochlorine pesticides record table 70
Table D. 1 Marine Biological Sample PCBs Analysis Table 74 records
Foreword
All technical content in this section is mandatory.
GB 17378 "marine monitoring" is divided into seven parts.
--- Part 1. General;
--- Part 2. Data processing and analysis of quality control;
--- Part 3. Sample collection, storage and transport;
--- Part 4. Seawater analysis;
--- Part 5. Sediment analysis;
--- Part 6. Analysis of the organism;
--- Part 7. Ecological survey of offshore pollution and biological monitoring.
This section GB of Section 617 378, instead of GB 17378.6-1998 "marine monitoring Part 6. organism minutes
Analysis. "
This section compared with GB 17378.6-1998 main changes are as follows.
--- Measurement project, methods and detection limits adjusted to "informative appendix" (1998 edition Chapter 5; this edition of Appendix B);
--- Increasing the total mercury "atomic fluorescence assay" (see 5.1);
--- Cancel the total mercury "dithizone spectrophotometry" (1998 version 6.2);
--- Increased arsenic "atomic fluorescence assay" (see 11.1);
--- Modified flameless atomic copper, lead and cadmium absorption spectrophotometry, adjusted to "copper, lead and cadmium continuous assay" (1998
Edition of 7.1,8.1,9.1; this edition 6.1,7.1,8.1);
--- Canceled copper "diethyl dithiocarbamate spectrophotometry" (1998 edition 7.4);
--- Canceled the lead "dithizone spectrophotometry" (1998 edition 8.3);
--- Canceled cadmium "dithizone spectrophotometry" (1998 edition 9.3);
--- Canceled zinc "dithizone spectrophotometry" (1998 edition 10.3);
--- Modify the "fluorescence spectrophotometry" (1998 edition Chapter 14; Chapter 13 of this edition) petroleum hydrocarbons;
--- Revise and improve various test methods of recording and adjust the table as "normative appendix" (see Appendix A);
--- Increased organochlorine pesticides "capillary gas chromatography" (see Appendix C);
--- Increased PCBs "capillary gas chromatography" (see Appendix D).
Appendix A of this section is normative appendix, Appendix B, Appendix C and Appendix D is an informative annex.
This part by the State Oceanic Administration.
This part of the National Standardization Technical Commission for Oceanography (SAC/TC283) centralized.
This section drafted by. National Marine Environmental Monitoring Center.
The main drafters of this section. mountain - foot plain, Xuheng Zhen, Yu Tao, Heguang Kai, Shang Longsheng, Zhaoyun Ying, Sun Qian, Han Dragon, Guan Tao Ming Ong Jian Guo,
Xukun Can, Zhang Chunming, Chenwei Yue, Hong Jun-chao, Chen Banglong.
This part of the standard replaces the previous editions are.
--- GB 17378.6-1998.
Marine monitoring Part 6. Analysis of the organism
1 Scope
This part of GB 17378 specifies the method for determination of marine organisms harmful substance residues mussels, shrimp and fish, and the samples were collected
Collection, transportation, storage, pretreatment and measurement results of computing technical requirements.
This section applies to marine life pollution investigation and monitoring of oceans, offshore and coastal waters.
2 Normative references
The following documents contain provisions which, through reference in this Part of GB 17378, constitute provisions of this part. For dated reference documents
Member, all subsequent amendments (not including errata content) or revisions do not apply to this section, however, encouraged to reach under this section
Parties to research agreement to use the latest versions of these documents. For undated reference documents, the latest versions apply to this
section.
GB 17378.3 specification for marine monitoring Part 3. Sample collection, storage and transportation
GB 17378.4 specification for marine monitoring Part 4. Seawater Analysis
GB 17378.5 specification for marine monitoring Part 5. Sediment analysis
3 Terms and Definitions
The following terms and definitions apply to this part of GB 17378.
3.1
The solvent was evaporated to a small volume (0.2mL ~ 0.3mL), leaving the residue was moist state.
3.2
Metering vessel volume mark.
[GB 17378.5-2007, Definition 3.1]
4 General Provisions
4.1 Collection and preparation of samples
4.1.1 Sample types
Shellfish, shrimp and fish. Shellfish gathering R.philippinarum general, clams, corners clams, blue mussel, Perna viridis, clam, razor clam, oyster capuchin
Oyster and so on.
4.1.2 Reagents
4.1.2.1 deionized or distilled water equivalent, the trace metal content should be below the detection limit of the analytical method, or were not contaminated seawater.
4.1.2.2 synthetic detergent.
4.1.3 instruments and equipment
Instruments and equipment are as follows.
--- Plastic freezer. with ice packs. When mussels for storage and transportation, should have a bottom grid, to avoid sample is immersed in water;
---refrigerator;
--- Cryogenic refrigerator;
--- Plates and plastic ruler. for length measurement;
--- Plastic knives;
--- Glass or ceramic dish. Preparation of samples;
--- Tweezers. plastic products or other suitable materials;
--- High-density polyethylene bags and plastic containers. you Save for frozen samples, before loading the sample, the application of synthetic detergent wash with distilled water
Wash;
--- Analytical balance. a sense of the amount of 0.1mg;
--- Plastic bottle;
--- Blade. for collecting samples;
--- Plastic buckets. capacity 20L ~ 50L;
--- Large metal knife. no rust, cut the fish tissue for use;
--- Homogenizer. stainless steel or other suitable material products;
--- Weighing bottle. Capacity 50mL;
--- Electric oven;
--- Oven;
--- Freeze-drying equipment.
4.1.4 Sampling and Transport
4.1.4.1 Preparations
Cleaning freezers synthetic detergent (see 4.1.2.2), high density polyethylene bags, plastic sheeting and feet, large metal knives, scrapers, and then steamed
Distilled water or seawater (see 4.1.2.1) rinse.
4.1.4.2 mussel samples collected
Mussel samples collected by the cleaning blade from its attachments.
Select a sufficient number of intact mussels stored in the freezer. For long-distance transport (hot days over 2h), should be filled in plastic sample mussels
Barrel, the clean sea water collected at the scene showered on mussels, samples were kept wet state but can not be immersed in water.
If the sample shall be carried out after 24h samples can be stored in the mussel-like high-density plastic bag, press out the air bag, tie the bag or
Sealing, this bag and the sample labels together into a polyethylene bag and sealed, stored in cryogenic freezer.
4.1.4.3 sized shrimp and fish samples were collected
Required to select a sufficient number of intact biological samples into a clean polyethylene bag, the bag should be prevented punctured. Out of the air bag,
Tie the bag or heat sealing, this bag and the sample labels together into another polyethylene bag, and sealed, cold storage. If the storage period is not too long
When (hot days, no more than 48h), refrigerators or freezers can be used to store samples.
4.1.4.4 Large fish samples were collected
Measure and write down the kind of fish fork length, weight and gender.
With a lower metal knife clean at least 100g of muscle tissue, the thickness of at least 5cm, the sample handling, removal of stains or visceral part. Deposit
In clean polyethylene bag, and seal out air, this bag and the sample labels together into another polyethylene bag, sealed in a deep freezer
In storage. If the retention time is not too long (hot days, no more than 48h), available fridge or freezer storage is a sample.
4.1.4.5 Transport of samples
After sample collection, if the long-distance transport, should sample into boxes (or plastic bucket), a package of sample should live without clean sea
Washout sprinkled on the sample, the sample holding wet state (can not be immersed in water); if the sample should be carried out after 24h samples, the sample can be placed
Polyethylene bag, press out the air bag, tie the bag. This together into bags and sample tags another polyethylene bags (or clean wide mouthed glass
Glass bottle), the sealing, frozen. Other Executive in accordance with the provisions of GB 17378.3.
4.1.5 Sample preparation
4.1.5.1 Preparations
When necessary, frozen samples in a refrigerator (-2 ℃ ~ 4 ℃) to stand overnight, so that part of thaw for slices.
Wash with synthetic detergent (see 4.1.2.2) plastic knives, dishes, forceps, plastic sheeting and feet and weighing of plastic film with distilled water or clean seawater
(See 4.1.2.1) rinse. Table cover washed plastic film. Synthetic detergent (see 4.1.2.2) carefully wash their hands after using steam
Distilled water or clean seawater (see 4.1.2.1) rinse.
4.1.5.2 shellfish sample preparation
Plastic shell with a plastic knife or brush to remove all external attachments.
With distilled water or clean seawater (see 4.1.2.1) rinsing each individual sample, let the natural flow of dry, pull the foot wire. With the balance, said individual
Total weight, and note the weight.
With another knife inserted into the plastic foot stretch silk exports, cutting the muscle closed and open shells.
With distilled water or clean seawater (see 4.1.2.1) to wash the soft tissue inside the shell, remove the soft tissue with a plastic knife and tweezers, let the water do.
Single individual samples. the soft tissue into the plastic container weighed, reweighed, note the fresh weight. Tightly closed and labeled. Measured with a ruler
Shell and record length.
More individual samples. the steps above to the soft tissue of at least 10 individuals into a known weight of the plastic container, weighing, note the fresh weight.
In homogenized homogenized samples, homogenized sample back in a plastic container, and then weigh and record the total weight, calculated homogenized sample weight. Paste sample
label.
Each individual organism size should be similar, and their individual lengths were measured and the total weight before removing biological tissue.
4.1.5.3 shrimp sample preparation
4.1.5.3.1 single individual samples
Long body with a ruler shrimp, shrimp-like film on the said polyethylene, weighing, note length, and fresh weight.
The chest and abdomen and head and tail separated by a plastic knife, carefully remove the viscera from the abdomen. Total removal of the leg. Turn down the abdomen with plastic
A stripper knife along the outer edge of the abdominal incision, remove the inside of the outer armor with plastic forceps and discarded.
Another with the plastic knife loose abdominal muscles, and muscle removed with tweezers.
Check the gonads, records identified gender.
Tweezers muscle moved plastic container, weighed and the fresh weight. Tightly closed containers, marked with numbers. The several containers together into the same
Plastic bag, together with sample registration list, knot it tightly, cold refrigerator.
4.1.5.3.2 more individual samples
Samples were prepared according to the method described above, carefully recording each individual length, fresh weight, abdominal muscle weight and gender. Each sample shall comprise six to
On the same sex, similar to the size of individual muscles. The samples were homogenized into a homogenizer abdominal muscles, known weight into a plastic container lid
Tight, marked with numbers, weighing, note the fresh weight and other data.
Several plastic containers in the same plastic bag, along with sample registration list, knot it tightly and stored at low temperature freezer.
4.1.5.4 Sample Preparation sized fish
4.1.5.4.1 single individual samples
Fish fork length measurements and said sample in a polyethylene film and weighed. Identification of gonadal sex, write down the fork length and weight.
With distilled water or clean seawater (see 4.1.2.1) washing the fish-like, it would be on the bench with a plastic knife cut pectoral and dorsal fin cutting attachment
Nearly from head to tail skin.
In the vicinity of the gill and tail, across all fish cut back; abdomen, sides and rear of each gill cut back. Only four knives cut in the side of the fish, and not
Cut too deep, so as not to cut offal, meat contamination.
Tweezers skin and meat separation, the outer skin to guard against contamination of meat.
The plastic knife to separate the muscles and spine with another, and tweezers to remove the muscles. Sheng will be organized in a plastic container, weighed and recorded
weight.
If not satisfy muscle mass analysis of the amount of the side, the other side of the muscle to take supplements.
Tightly closed container, label or mark, make a record and stored at low temperature freezer.
4.1.5.4.2 more individual samples
Carefully recording each individual body length, fresh weight, muscle weight. Identification of sex. The number of individuals should not be less than 6, and should be the same sex, same size.
Homogenized by a homogenizer fish tissue will be homogenized sample into a known weight of the plastic container, tightly closed, labeled and weighed, homogenized sample weight write down
And other data. Placed in cold storage in the refrigerator.
4.1.5.5 Large fish sample preparation
If necessary, the samples collected at the scene placed -2 ℃ ~ 4 ℃ refrigerator overnight, so that part in order to thaw the slice.
With distilled water or clean seawater (see 4.1.2.1) and washed fish samples. The fish samples in a clean work surface, remove the remnants of skin and bone, with
Plastic knife to the surface, and then the other to repeat a plastic knife, leaving from pollution muscle tissue. The muscle tissue placed in a plastic container
Vessel, capped, labeled, weighed, and the data recorded in the record sheet, stored in a deep freezer in the sample.
4.1.5.6 dry sample preparation
The portion of the fresh sample drying step according to 4.1.6.1 or 4.1.6.2, the calculation of wet and dry than to correct moisture content. After drying the sample with
Agate mortar and pestle, all over 80 mesh and 100 mesh (180μm ~ 154μm) nylon screen for trace element analysis.
4.1.6 Determination of the dry weight
4.1.6.1 Drying
The weighing bottle placed in an oven at 105 ℃, 2h, remove the weighing bottle and placed in the dryer to cool 30min.
Cover caps, weighed with an analytical balance, note the weight. Take 5g ~ 10g of the biometric sample preparation in the weighing bottle, cover caps, and then said
Weight (± 0.5mg) and note the weight.
The weighing bottle containing the sample into the semi-open lid 105 ℃ oven, removed after 24h, placed in the dryer to cool 30min. After the cover cap
Weigh and record the weight alleged.
Repeat the drying operation, the drying to the weight before and after the two is less than 0.5% of the total weight. Wet and dry weight ratio calculation.
4.1.6.2 lyophilized
High levels of lipids in biological samples, can not be dried to constant weight, the application freeze-dried. Weigh accurately 1g ~ 2g the biometric system
Preparation of the sample in a clean container freeze-dried samples, weighed after the first freeze-drying 24h. Again lyophilized 24h, reweighed. twice
Weigh weight difference should be less than 0.5% by weight of the total. Otherwise, it should continue to be dried to meet the requirements. Wet and dry weight ratio calculation.
4.1.7 Precautions
The provisions should note the following.
--- Mussels collected near the laboratory, there is no special transport and storage problems. When transported to the laboratory, samples should be ventilated with mussels
Seawater remains moist. Inter collected from intertidal mussels can survive in air for 24h. Mussels should not be placed in water transport;
--- After hand washing, not touching anatomy, should wear gloves; if conditions permit, preparation and sample preparation shall be in a clean strip
Element is carried out;
--- When multiple individual sample preparation, should take the same sex, similar to the size of individual organisms. Before removing the soft tissue should be measured separately for each
Body length and weight of the body;
--- Sample before digestion, the vessel containing the total weight of the sample and the weight of the storage time of the comparison, can be found in the samples during storage if
weightlessness;
--- Trace metal content in different parts of the muscle may differ, so the actual sample information should be recorded in detail as far as possible;
--- A biological sample for organochlorine pesticides and petroleum hydrocarbons measured, sample collection and pre-treatment equipment and reagents make the appropriate corresponding changes
Change, should avoid the use of plastic containers containing halogenated reagents;
--- Determination of total mercury and organisms harmful organisms, not dried sample application, the application of wet sample measurement, the results are still dry sample analyte
Content to represent.
4.2 regulations and requirements
4.2.1 Analysis of samples drying. drying temperature and time are not specified, refer to 105 ℃ ± 1 ℃, drying 2h.
4.2.2 Standard Solution, all pipettes and flasks test should be performed or capacity correction.
4.2.3 Unless otherwise stated, the purification of the container are to (1 + 3) soaked with a solution of nitric acid 2d ~ 3d after carefully with deionized water shower
Wash, dry spare.
4.2.4 pH value unless otherwise indicated measurement methods, are available a wide range of pH test paper or precision measurements.
4.2.5 To check the quality of the analysis results, samples should be analyzed by a group of random selection of inspection samples in Table 1, respectively, bagging and other series like numbers, the base
This kind of cross-check sample analysis testers, determined according to the following requirements.
--- Sample checks of the same kind of basic measurement items;
--- When the number of samples analyzed more basic kind of check samples can be tested should not be scheduled in the same batch;
--- Test results are listed in Table 2 twin sample relative deviation of analytical quality control. When a two-item test sample test results is greater than the super slip
30% of this batch of basic samples should be fully re-entry to the test sample, said determination;
--- If the above still-tolerance conditions, analysis and testing should be carefully checked analyze the reasons (such as the preparation of the environmental quality standard solution, the
There are no unusual circumstances, etc.) with the equipment, and then measured the sample batch (basic sample and check samples) of;
--- When a test sample test results exceed double entry error rate of less than 30%, the sample should be re-called ultra-poor samples were measured until a new measurement results
If qualified so far. A parallel double sample mean reported results;
--- Analysis of each batch of samples (20 or so) should be inserted 2 to 3 certified reference material sample (separate numbers) to test whether the system
Systematic error.
Table 1 Analysis of samples taken from the check-like proportions
The number of samples analyzed/a < 10 10-30> 30
Check sample extraction ratio /% 504 030
Table 2 parallel double sample relative deviation table
The results where the magnitude 10-410-510-6 10-710-810-9
Relative deviation allowable limit /% 4815203040 computing. | AB | A + B × 100
4.3 Description
4.3.1 various chemical density (ρ) refers to the 20 ℃, mass divided by volume, in units of g/mL.
4.3.2 desiccant when not indicate a specific name, refer to color gel.
4.3.3 concentration of the standard elements are formulated refers to the concentration of the element.
4.3.4 does not specify solvent solution is an aqueous solution.
5 Total Mercury
5.1 Atomic Fluorescence Spectrometry
5.1.1 Scope and Application
This method is applicable to the determination of total mercury in marine organisms.
This method is a method of arbitration.
5.1.2 The principle of the method
In nitric acid - perchloric acid digestion system, the total amount of mercury in the organism into mercury ions into solution. With potassium borohydride as a reducing agent
Solution of mercury ions to mercury vapor. Argon as a carrier gas of atoms of mercury vapor into the atomic fluorescence spectrometer of atomic reactor, with special
Species mercury hollow cathode lamp as the excitation source, the determination of mercury atomic fluorescence intensity.
5.1.3 Reagents and preparation
5.1.3.1 nitric acid (HNO3). ρ = 1.42g/mL, pure class distinctions.
5.1.3.2 perchloric acid (HClO4). pure class distinctions.
5.1.3.3 hydrochloric acid (HCl). ρ = 1.19g/mL, pure class distinctions.
5.1.3.4 oxalic acid (H2C2O4 · 2H2O).
5.1.3.5 potassium borohydride (KBH4).
5.1.3.6 potassium hydroxide (KOH). pure class distinctions.
5.1.3.7 nitric acid solution (1 + 19). 1 The volume ...
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