This part of GB17378 specifies the analysis methods for seawater monitoring projects, and puts forward technical regulations and requirements for the sample collection, storage, transportation, and calculation of measurement results of seawater analysis. This part is applicable to oceans, offshore, estuaries, and mixed salt and fresh waters. It can be used for marine environmental monitoring, routine water quality monitoring, environmental pollution investigation and monitoring in nearshore shallow waters, as well as emergency special investigation and monitoring of marine dumping, dredged materials, red tides, and marine pollution accidents, and marine environmental investigation and monitoring related to the ocean. GB 17378.4-2007 Marine Monitoring Specification Part 4: Seawater Analysis GB17378.4-2007 Standard Download Decompression Password: www.bzxz.net
This part of GB17378 specifies the analysis methods for seawater monitoring projects, and puts forward technical regulations and requirements for the sample collection, storage, transportation, and calculation of measurement results of seawater analysis. This part is applicable to oceans, offshore, estuaries, and mixed salt and fresh waters. It can be used for marine environmental monitoring, routine water quality monitoring, environmental pollution investigation and monitoring in nearshore shallow waters, as well as emergency special investigation and monitoring of marine dumping, dredged materials, red tides and marine pollution accidents and marine environmental investigation and monitoring related to the ocean.
All technical contents of this part are mandatory.
GB17378 "Marine Monitoring Specification" is divided into seven parts:
--- Part 1: General Principles;
--- Part 2: Data Processing and Analysis Quality Control;
--- Part 3: Sample Collection, Storage and Transportation;
--- Part 4: Seawater Analysis;
--- Part 5: Sediment Analysis;
--- Part 6: Organism Analysis;
--- Part 7: Ecological Investigation and Biological Monitoring of Nearshore Pollution.
This part is Part 4 of GB 17378 and replaces GB 17378.4-1998 “Ocean Monitoring Specifications Part 4: Seawater Analysis”.
Compared with GB17378.4-1998, the main changes in this part are as follows:
--- Water sampling, storage and transportation are adjusted to normative appendix (4.3 of 1998 edition; Appendix B of this edition);
--- Detection limit is adjusted to informative appendix (Chapter 5 of 1998 edition; Appendix C of this edition);
--- Atomic fluorescence determination of mercury is added (see 5.1);
--- Dithizone spectrophotometry of mercury is cancelled (6.2 of 1998 edition);
--- Flameless atomic absorption spectrophotometry for copper, lead and cadmium is revised and adjusted to continuous determination of copper, lead and cadmium (7.1, 8.1, 9.1 of 1998 edition; 6.1, 7.1, 8.1 of this edition);
--- The sodium diethylaminodithiocarbamate spectrophotometric method for copper (7.4 of the 1998 edition) has been cancelled;
--- The dithizone spectrophotometric method for lead (8.4 of the 1998 edition) has been cancelled;
--- The dithizone spectrophotometric method for cadmium (9.4 of the 1998 edition) has been cancelled;
--- The dithizone spectrophotometric method for zinc (10.3 of the 1998 edition) has been cancelled;
--- The atomic fluorescence determination method for arsenic has been added (see 11.1);
--- The cyclohexane extraction fluorescence spectrophotometric method for oils has been modified (14.1 of the 1998 edition; 13.1 of this edition);
--- The freon-cyclohexane extraction system fluorescence spectrophotometric method (14.2 of the 1998 edition) has been cancelled;
---Transparency-Visual method was changed to Transparency-Transparent disk method (23.1 of 1998 edition; 22 of this edition);
---The pH colorimetric method for pH was cancelled (27.2 of 1998 edition);
---The temperature-salinity-depth (CTD) method for salinity was added (see 29.2);
---The instrumental method for total organic carbon was added (see 34.1);
---The potassium persulfate oxidation method for total phosphorus was added (see Chapter 40);
---The potassium persulfate oxidation method for total nitrogen was added (see Chapter 41);
---The flameless atomic absorption spectrophotometric method for nickel was added (see Chapter 42);
---Appendix A was modified and improved and adjusted to a normative appendix (Appendix A of 1998 edition; Appendix A of this edition);
---Appendix B is adjusted to an informative appendix (Appendix B of the 1998 edition; Appendix D of this edition).
Appendices A and B of this part are normative appendices, and Appendix C and Appendix D are informative appendices.
This part is proposed by the State Oceanic Administration.
This part is under the jurisdiction of the National Technical Committee for Marine Standardization (SAC/TC283).
Drafting unit of this part: National Marine Environmental Monitoring Center.
Main drafters of this part: Ma Yongan, Xu Hengzhen, Yu Tao, He Guangkai, Zhao Yunying, Zhang Guoguang, Shang Longsheng, Sun Qian, Wu Zhiqing, Chen Shumei, Han Gengchen, Guan Daoming, Wang Jianguo, Zhang Chunming, Xu Kuncan, Chen Weiyue, Chen Banglong, Zhan Xiuwen. The
previous versions of the standards replaced by this part are:
---GB17378.4-1998.
The clauses in the following documents become clauses of this part through reference in this part of GB 17378. For all dated referenced documents, all subsequent amendments (excluding errata) or revisions are not applicable to this part. However, parties to agreements based on this part are encouraged to study whether the latest versions of these documents can be used. For all undated referenced documents, the latest versions are applicable to this part.
GB/T12763.2 Specifications for marine surveys Part 2: Marine hydrological observations
GB/T12763.4 Specifications for marine surveys Part 4: Marine chemical element surveys
GB17378.2 Specifications for marine monitoring Part 2: Data processing and analysis quality control
GB17378.3 Specifications for marine monitoring Part 3: Sample collection, storage and transportation
HY/T07-1992 Inversion temperature table
Foreword V
1 Scope 1
2 Normative references 1
3 Terms and definitions 1
4 General provisions 1
5 Mercury 2
5.1 Atomic fluorescence spectrometry 2
5.2 Cold atomic absorption spectrophotometry 4
5.3 Gold capture cold atomic absorption spectrophotometry 6
6 Copper 10
6.1 Flameless atomic absorption spectrophotometry (continuous determination of copper, lead and cadmium) 10
6.2 Anodic stripping voltammetry (continuous determination of copper, lead and cadmium) 12
6.3 Flame atomic absorption spectrophotometry 13
7 Lead 15
7.1 Flameless atomic absorption spectrophotometry 15
7.2 Anodic stripping voltammetry 15
7.3 Flame atomic absorption spectrophotometry 15
8 Cadmium 17
8.1 Flameless atomic absorption spectrophotometry 17
8.2 Anodic stripping voltammetry 17
8.3 Flame atomic absorption spectrophotometry17
9 Zinc19
9.1 Flame atomic absorption spectrophotometry19
9.2 Anodic stripping voltammetry21
10 Total chromium22
10.1 Flameless atomic absorption spectrophotometry22
10.2 Diphenylcarbazide spectrophotometry24
11 Arsenic26
11.1 Atomic fluorescence spectrophotometry26
11.2 Arsine-silver nitrate spectrophotometry28
11.3 Hydride generation atomic absorption spectrophotometry30
11.4 Catalytic polarography32
12 Selenium35
12.1 Fluorescence spectrophotometry 35
12.2 Diaminobenzidine spectrophotometry 37
12.3 Catalytic polarography 39
13 Oils 42
13.1 Fluorescence spectrophotometry 42
13.2 Ultraviolet spectrophotometry 44
13.3 Gravimetric method 45
14 666, DDT --- Gas chromatography 47
15 Polychlorinated biphenyls --- Gas chromatography 50
16 Dieldrin --- Gas chromatography 54
17 Active silicates 57
17.1 Silico-molybdenum yellow method 57
17.2 Silico-molybdenum blue method 59
18 Sulfide 60
18.1 Methylene blue spectrophotometry 60
18.2 Ion selective electrode method 64
19 Volatile phenol --- 4-aminoantipyrine spectrophotometry 67
20 Cyanide 70
20.1 Isonicotinic acid-pyrazolone spectrophotometry 70
20.2 Pyridine-barbituric acid spectrophotometry 73
21 Water color --- colorimetric method 75
22 Transparency --- transparent disk method 76
23 Anionic detergent --- methylene blue spectrophotometry 76
24 Smell and taste --- sensory method 78
25 Water temperature 79
25.1 Surface water temperature meter method 79
25.2 Inverted thermometer method 80
26 pH-pH meter method 83
27 Suspended matter---gravimetric method 88
28 Chloride---argentometric titration method 91
29 Salinity 92
29.1 Salinometer method 92
29.2 Temperature-salinity-depth (CTD) method 95
30 Turbidity 95
30.1 Turbidimeter method 95
30.2 Visual turbidimetry 96
30.3 Spectrophotometric method 98
31 Dissolved oxygen --- iodine titration method 99
32 Chemical oxygen demand --- alkaline potassium permanganate method 101
33 Biochemical oxygen demand 103
33.1 Five-day culture method (BOD5) 105
33.2 Two-day culture method (BOD2) 103
34 Total organic carbon 105
34.1 Total organic carbon instrumental method 105
34.2 Potassium persulfate oxidation method 107
35 Inorganic nitrogen 109
36 Ammonia 109
36.1 Indophenol blue spectrophotometric method 109
36.2
38 Nitrite --- Naphthylethylenediamine Spectrophotometry 113 ||tt ||
38 Nitrate 115 || tt||
38.1 Cadmium column reduction method 115
38.2 Zinc-cadmium reduction method 117
39 Inorganic phosphorus 117
39.1 Phosphomolybdenum blue spectrophotometry 117
39.2 Phosphomolybdenum blue extraction spectrophotometry 119
40 Total phosphorus --- Potassium persulfate oxidation method 120
41 Total nitrogen --- Potassium persulfate oxidation method 121
42 Nickel --- Flameless atomic absorption spectrophotometry 121
Appendix A (Normative Appendix) Record Sheet 123
Appendix B (Normative Appendix) Water Sample Collection, Storage and Transportation 156
Appendix C (Informative Appendix) Method Detection Limit 160
Appendix D (Informative Appendix) Preparation of working auxiliary standard seawater 162
Figure 1 Cold atomic absorption mercury measuring device 5
Figure 2 Gold capture cold atomic absorption mercury measuring device 8
Figure 3 Arsenic generation and absorption device 29
Figure 4 Alkaline hydrolysis reflux device 52
Figure 5 Hydrogen sulfide aeration device 63
Figure 6 Surface water temperature table 79
Figure 7 Suspended matter measurement operation flow 89
Figure 8 Filtration system 89
Figure 9 Carbon dioxide measurement device 108
Table 1 Salinity correction value table 58
Table 2 Smell and taste intensity level 78
Table 3 Main specifications of primary and secondary temperatures 80
Table 4 Counter correction value (α) table (for hanging water sampler) 81
Table 5 pH values ​​of standard buffer substances at 0℃~45℃85
Table 6 Temperature correction value α (tm-tw) for pH determination Table 86
Table 7 Pressure correction coefficient β for pH determination Table 86
Table 8 pH~αH+ conversion table 87
Table 9 Salt error correction coefficient table 111
Table A.1 Data record of standard (working) curve for water quality sample analysis (atomic fluorescence method) 123
Table A.2 Data record of water quality sample analysis (atomic fluorescence method) 124
Table A.3 Data record of standard (working) curve for water quality sample analysis (spectrophotometry) 125
Table A.4 Data record of water quality sample analysis (spectrophotometry) 126
Table A.5 Water quality sample analysis standard (working) curve data record (non-flame atomic absorption spectrophotometry) 127
Table A.6 Water quality sample analysis record (non-flame atomic absorption spectrophotometry) 128
Table A.7 Water quality sample analysis record (anodic stripping voltammetry) 129
Table A.8 Water quality sample analysis standard (working) curve data record (flame atomic absorption spectrophotometry) 130
Table A.9 Water quality sample analysis standard (working) curve data record (catalytic polarography) 131
Table A.10 Water quality sample analysis record (catalytic polarography) 132
Table A.11 Water quality sample analysis standard (working) curve data record (fluorescence spectrophotometry) 133
Table A.12 Water quality sample analysis record (fluorescence spectrophotometry) 134
Table A.13 Water sample oil analysis record (gravimetric method) 135
Table A.14 Water sample 666, DDT, dieldrin analysis record (gas chromatography) 136
Table A.15 Water sample PCB analysis record (gas chromatography) 137
Table A.16 Water sample nutrient salt analysis record (spectrophotometry) 138
Table A.17 Water sample sulfide analysis standard (working) curve data record (sulfide ion selective electrode method) 139
Table A.18 Water sample sulfide analysis record (sulfide ion selective electrode method) 140
Table A.19 Surface thermometer observation record table 141
Table A.20 Water temperature observation record table 142
Table A.21 Water temperature observation record table 143
Table A.22 pH measurement record (method) 144
Table A.23 Seawater suspended matter analysis record (gravimetric method) 145
Table A.24 Water quality sample chloride analysis record (argentometric titration method) 146
Table A.25 Water quality sample salinity measurement record (salinometer method) 147
Table A.26 Water quality sample turbidity analysis standard curve data record (method) 148
Table A.27 Water quality sample turbidity measurement record (method) 149
Table A.28 Water quality sample dissolved oxygen analysis record (iodine titration method) 150
Table A.29 Water sample chemical oxygen demand analysis record (alkaline potassium permanganate method) 151
Table A.30 5-day biochemical oxygen demand analysis record (5-day 20℃ incubation method) 152
Table A.31 Total organic carbon analysis record in seawater (instrumental method) 153
Table A.32 Marine environment monitoring water quality report 154
Table A.33 Water sampling record 155
Table B.1 Water sampling volume and storage 156
Table C.1 Detection limit of determination method 160

ICS 07.060
National Standard of the People's Republic of China
GB17378.4—2007
Replaces GR17378.4-1998
The specification for marine monitoring--Part 4: Seawater analysis
2007-10-18 Issued by
General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China and Standardization Administration of China
2008-05-01 Implementation
Normative references
3 Terms and definitions
General provisions
Fluorescence method,
E, 2 Cold atomic absorption spectrophotometry
5.3 Gold extraction cold atomic absorption spectrophotometry
Flameless atomic absorption spectrophotometry (continuous determination of copper, aluminum and) 6,2 and stripping voltammetry (continuous determination of copper, lead and zinc) 65. 3
Flame atomic absorption spectrophotometry
Non-flame atomic absorption spectrophotometry...7.2
Anodic stripping voltammetry
7.3 Flame atomic absorption spectrophotometry...8.
Non-flame atomic absorption spectrophotometry
8.2 Stripping voltammetry
8.3 Flame atomic absorption spectrophotometry
Flame atomic absorption spectrophotometry
0. 2 Anodic dissolution voltammetry
[0.1 Flameless tracer absorption spectrophotometry Benzene carbonyl spectrophotometry
Original light
Hydrogen nitrate silver spectrophotometry
Chemical polarography
Fluorescence spectrophotometry
Benzidine spectrophotometry
Catalytic polarography
13 Fluorescence spectrophotometry
CB 17378. 4—2007
GB 17378, 4—2007
Ultraviolet spectrophotometry
Heavy-dust method
Polynitrogen-containing tea
Dieldrin
Active silicate
Silica yellow method
Silica vanadium blue method
Sulfide
Gas chromatography
Gas chromatography
Gas chromatography
Industry currency basic monitoring Photometric method
Ion selective electrophoresis method
Volatilization
Mosin
1-aminoantipyrine spectrophotometric method
Nicotinoic acid-oxazolinone spectrophotometric method
Pyrrophthalic acid spectrophotometric method
Transparency
Colorimetric method
Transparent round blue method
Anion detergent| |tt||Smell and taste
Sensory method
Surface water wetness method
Thermostat method
Floating substance
Chloride
Heavy rat secret
Methylene blue spectrophotometry
Egg mullet titration
Saltometer method
Crystal-salinity depth meter (CTT) method
Turbidity|| tt||Turbidimeter method
National Vision Turbidimetry
Spectrophotometry
Iodometric method
Chemical oxygen demand
Biochemical oxygen demand
Alkaline potassium permanganate pool
Tuberculosis culture method (B))
Two-day culture method (B)L.)
Total organic carbon
Total organic carbon instrumental method||t t||Potassium persulfate oxidation method
Nine machine bombs
Indigo blue spectrophotometry
36.2 Algae salt oxidation method:
37 Nitrite-naphthylethylenediamine spectrophotometry38 Nitrate·
Pot reduction method
37.2 Zinc-tantalum reduction method
39 Inorganic phosphorus·
Phosphomolybdenum blue spectrophotometry
39.2 Phosphorus blue extraction spectrophotometry·
40 Total phosphorus·Persulfate oxidation method
41 Total nitrogen Potassium persulfate oxidation method·
12-line-free olefin atomic absorption spectrophotometry Appendix A (normative appendix) Record table
Appendix B (normative appendix)
Appendix ((informative appendix)
Appendix D (Informative Appendix)
Water sample collection, storage and transportation
Detection limit of the method
Preparation of working standard seawater
Cold atomic absorption mercury measuring device
Gold donation cold atomic absorption mercury measuring device
Arsine generation-absorption device
Alkaline hydrolysis flow device
Hydrogen sulfide aeration device
Surface water temperature loss
Suspended matter determination operation flow
Filtration system
Carbon dioxide determination device
Salinity correction table
Membranes and taste strength grades
Main specifications of card temperature
Counter correction value () table (for hanging water sampler) Table 0t---45℃Standardized pH value of buffer substances Table 6pll Determination of temperature correction value α (tm-t) Table 7pll Table of measured pressure correction coefficient β Conversion table of pI～a' Salt error correction coefficient table Water quality sample Water quality sample Water quality sample Water quality sample Water quality sample Water quality sample Water quality sample Water quality sample Water quality sample Water quality sample Water quality sample Analysis standard (working) West line data record (atomic fluorescence method) Analysis record (atomic fluorescence method) Analysis standard (working) ) curve data record (analysis record (
spectrophotometry)
spectrophotometry latent)
GB17378.4—2007
analysis standard (working) curve data record (flameless atomic absorption spectrophotometry) analysis record (flameless atomic absorption spectrophotometry) ·*analysis record (anodic stripping voltammetry)
analysis standard (T.working) curve data record (flame atomic absorption spectrophotometry) 127
GB 17378. 4-2007
A. Water quality samples
Water quality samples
Water quality samples
Water quality samples
Standard (working) curve data record (catalytic polarography) analysis record (catalytic spectroscopy)
Analysis standard (working) curve data record (fluorescence spectrophotometry) analysis record (fluorescence spectrophotometry)
Water quality sample oil analysis record (gravimetric method) Water quality sample 666, DI) T. Dieldrin analysis record (gas chromatography) Water quality sample B analysis record? (Gas chromatography). Water quality sample nutrients.
Analysis record (spectrophotometry)
Water sample sulfide analysis standard (.working) curve data record (sulfide ion selective electrode method) Water sample sulfide analysis record (sulfide ion selective electrode selection) Surface humidity meter observation record
Tide observation record sheet
Water temperature measurement record
iH determination record (
Seawater suspended matter analysis record (gravimetric method) Water sample chlorination analysis record (silver titration method) Water sample salt determination record (salinometer method) Water sample turbidity analysis standard curve data record (water sample turbidity determination record (
Water sample dissolved oxygen analysis record (iodine method) Water sample chemical hydrogen demand analysis record (alkali potassium permanganate method) 5H dust demand analysis record (5H 2:)℃ culture method) Total organic carbon analysis record in seawater (instrumental method) Marine environment monitoring water quality report
Water sample sampling record
Water sample sampling volume and preservation
Determination method detection limit
! -16
All technical contents of this part are mandatory. Foreword
GB17378 Marine Monitoring Specifications" is divided into two parts: Part 1: General deletion;
Part 2: Data processing and analysis quality control; Part 3: Sample collection, storage and transportation: Part 4: Swimming water analysis;
Part 5: Sediment analysis;
-Part 5 Organism analysis:
Part 7: Ecological investigation and biological monitoring of offshore pollution, GB 17378. 4—2007
This part is the first part of (G1317378. Replaces (B17378, -1998 Ocean Monitoring Specification Part 4: Seawater Analysis). Compared with CB173/8.1-1938, this part has the following changes: Water samples are collected,Storage and transportation were adjusted to normative appendix (1.3 of 1998 edition; Appendix B of this edition); detection limit was adjusted to scientific appendix (Chapter 5 of 1998 edition, Appendix () of this edition); the widely used atomic fluorescence determination method was added (see 1); the widely used disulfide spectrophotometric method (6.2 of 1998 edition) was cancelled: the flameless atomic absorption spectrophotometric method for steel, lead and pot was modified and adjusted to the continuous determination method for lead and copper (7.1, 8.1, 1.1 of 1998 edition; 6.1, 7.1, 8.1 of this edition); the diaminothiocyanate spectrophotometric method for copper (198 edition, 1) was cancelled; the disulfide spectrophotometric method for lead (8.4 of 1998 edition) was cancelled; the double sulphuric spectrophotometric method for radiation (1998 edition) was cancelled. 9.1 of this edition): - The double flow trace spectrophotometry for zinc (19.3 of the 1918 edition) was cancelled and the atomic emission spectrophotometry for determination of the content of carbonyl alcohol was added (see 1.［); - The cyclohexane extraction fluorescence spectrophotometry for oils was modified (11.1 of the 1998 edition and 13.1 of this edition); - The fluorine-carbon spectrophotometry with cyclohexane extraction system was cancelled (14.2 of the 1998 edition); - The transparency 11-view method was modified to the transparency transparent circle method (23.1 of the 1998 edition and 22 of this edition); - The colorimetric method of FI1 (27.2 of the 1998 edition) was eliminated; - The determination method of salinity by tidal salt depth instrument (CI1) was added (see 29.2); - The determination method of total organic carbon by total organic carbon analyzer was added (see 34.1); - The simplified determination method of total phosphorus by persulfate was added (see 41); - The determination method of total nitrogen by hydrogen persulfate was added (see 41); - The determination method of nickel by flame absorption spectrophotometry was added (see 42); - Appendix A was revised and improved and adjusted to the current normative appendix (1998 edition) Appendix A of the 1918 edition: Appendix A of this edition); Appendix B is adjusted to an informative appendix (Appendix 3 of the 1918 edition; Appendix 1 of this edition)) Appendix A and Appendix B of this part are normative appendices, and Appendix and Appendix B are informative excerpts. This part was proposed by the State Oceanic Administration. This part was drafted by the National Marine Standardization Technical Committee (SAC/TC283). Unit: National Marine Environmental Monitoring Center. The main drafters of this part; Ma Shui'an, Xu Jiezhen, Yu Tao, He Guangkai, Zhao Yunying, Zhang Guoguang, Shang Longniu, Sun Qian, Huo Zhiqing, Chen Shumei, 1 Scope
Ocean blue measurement specification
Part 4: Seawater analysis
GB 17378. 4—2007
This part of GB17378 specifies the analysis methods for seawater monitoring projects, and puts forward technical regulations and requirements for the collection, purchase, transportation, and calculation of test results of seawater analysis samples. This part is applicable to oceans, offshore, estuaries, and mixed freshwater areas, and can be used for marine environmental monitoring, routine water quality monitoring, environmental pollution investigation and monitoring in shallow waters, and emergency special investigation and monitoring of marine dumping, dredged materials, red traces, and marine pollution accidents, as well as marine environmental investigation and monitoring related to the ocean.
2 Normative references
The clauses in the following documents become the clauses of this part through reference in this part of CB17378. For any referenced document with a date, all subsequent amendments (excluding errata) or revisions are not applicable to this part. However, the parties to an agreement based on this part are encouraged to study whether the latest versions of these documents can be used. For any referenced document without a date, the latest versions are applicable to this part.
GB/712763.2 Marine survey specifications Part 2: Marine hydrological observation CB/T1276:3.4 Marine survey specifications Part 1: Marine chemical element survey GB317378.2 Marine monitoring specifications Part 2: Data processing and analysis quality control GB1737S.3 Marine monitoring specifications Part 3: Sample collection, storage and transportation IY/07-1992 Inverted temperature table
3 Terms and definitions
The following terms and definitions apply to this part of GB1317378. 3.1
Filtered water sampleFiltered water sampleWater filtered with 0.4Bμm fiber filter membrane. 3.2
Standard line
Graduation line for measuring the volume of a container:
4 General provisions
4.1 Purification and treatment of reagents, solvents and filter membranes4.1.1 Purification of ammonia water by equal diffusion method: Place the containers containing ammonia water and high-purity water separately on a glass desiccator partition or under a partition, and place them in a sealed manner. The separation time depends on the temperature and is about 2 weeks. 4.1.2 Purification of chloroform and carbon tetrachloride: The newly sealed solvent can be simply treated. That is, add 20inL of hydrochloric acid solution (volume fraction: 1:1) to each liter of reagent, shake and wash in the separatory to remove the aqueous phase, then wash with pure water and filter with dried filter paper. If the waste solvent is to be recycled or still unqualified after being treated by the above method, the following method shall be used instead: Pour the solvent into a distillation bottle half full, add an appropriate amount of sodium sulfate solution (volume fraction 1C%) to cover the upper layer, perform the first distillation, then transfer it to a clean distillation bottle, add solid calcium oxide for the second distillation, discard a small amount of the initial distillate, collect the distillate and store it in a brown bottle. If the solvent is chloroform, GK 17378.4-2007
[Clean water ethanol can be added to increase the stability of H, 4.1.3 (.451rml fiber filter: Use stainless steel tweezers with polyethylene film to hold the edge of the filter membrane, and vertically downwardly apply 0.5 mol/1.0 solvent for at least 12 hours. Rinse with pure water until neutral, seal and set aside. 4.2 Instructions
4.2.1 Subtraction of standard blank (1,) and analytical blank (4) 4.2. 1. 1 When A1=A2 (i.e. the determination steps of the standard series and the water sample are the same), both do not need to be eliminated, i.e. A1 does not subtract A2; A2 does not subtract A3, and the calibration curve is drawn or the curve is checked. This is only applicable to the same batch: if the blank value (A1 and A2) is very stable, the calibration curve can be used again. Note: Absorbance of water sample
Note 2: A1: Absorbance value of analytical cross-talk:
Note 3: Absorbance value of each point in the standard series. The concentration is the standard value. A.4.2. 1.2 When A1=A2, i.e. the determination steps of the standard series are omitted compared with the water sample, the curve must be drawn after A1=A2; 4w calibration curve is checked
4.2. 1. 3 The linear regression equation should be calculated according to the above provisions. 4.2.1.4 Atomic absorption, gas chromatography, electrochemical and other determination methods. Refer to the ". 4.2.2 Correction of salt error
Correction of salt error (error caused by different ion strength) should be made with pure seawater. If pure water is used, the correction factor will be given; some correction factors (such as silicon and nitrogen) are more passively affected by the environment and pure water, and the user should make necessary corrections based on the actual measured results.
4. 2.3 Correction of water sample volume Before measuring the water sample, if the volume of the water sample exceeds the above volume, perform volume correction according to the formula: Viv Output: V: Volume of water sample after correction, in milliliters (ml): V - original volume of water sample, in milliliters (ml): V - volume of water sample to be measured, in liters (ml) V - volume of added reagent solution, in milliliters (ml). 4.2.4 Verification of test method tt||Water leakage, salinity, water color, transparency, chlorine, chemical base, ammonia hypobromite method and other testing methods are equivalent to the classic methods at home and abroad. Most of its performance indicators are verified again. 4.2.5 Relative deviation limit between parallel samples and recovery rate of spiked natural samples. Repeat the relative deviation limit between parallel samples and recovery rate of spiked natural products. If the original method does not make a determination, it shall be carried out in accordance with the provisions of (B17378.2).
5.1 Atomic fluorescence method| |tt||5.1.1 Scope and application area
Applicable to the determination of mercury in seawater in ocean, nearshore and estuary areas. This method is an arbitration method.
5.1.2 Principle of the method
After the water sample is digested with sulfuric acid and potassium persulfate, the mercury ions are reduced to elemental mercury under the action of the reducing agent potassium borohydride. Fluorine gas is used as a carrier (the vapor is carried into the atomizer of the photometer in the future), and a special mercury hollow cathode lamp is used as the excitation light source to determine the fluorescence intensity of mercury.
5. 1. 3 Reagents and their preparation
5.1.3.1 Sulfur: process ultrapure-p-1.84g/ml.5.1.3.2 Nitric acid: high-grade pure.g-1.42/mL. Hydroxylamine hydrochloride (NHOII, HC1)
5. 1. 3. 33
5. 1.3. 4:
Potassium persulfate (K:S.0:)
5. 1. 3.5
Potassium borohydride (KBH),
5. 1, 3, 63
Potassium hydroxide (KOH): high grade pure,
5. 1. 3. 7
G:B 17378. 4—2007
Hydroxylamine hydrochloride solution (100 g/L): weigh 2 g of hydroxylamine hydrochloride (see 5.1.3.3) and dilute it to 250 ml of water, potassium persulfate solution 59 g/L): weigh E0R potassium persulfate (see 5.1.3.4) and dissolve it in water and dilute to 1900 ml. 1.5. 1.3.8
5.1.3.9 Sulfuric acid solution: slowly add 28 ml of sulfuric acid (see 5.1.3.1) to 500 ml of water under stirring and dilute to 1 (00 m)
5.1.3.10 Nitric acid solution (1-1 19): Slowly add 50 ml of nitric acid (see 1.3.2) to 100 mL of water. 5.1.3.11 K13H2O solution (6.05 mg/ml): Take 1 ml potassium hydroxide (5.1.3.6) and dissolve it in 260 ml water. Add 0.1% borohydride (see 5.1.3.5). Take 2 mL and dilute with water to 1 (0) ml. 5.1.3.12 Prepare standard solution for mercury (1.00 mg/ml): Accurately weigh 9.135 g of high-grade mercury chloride (HgCl, which has been dried in sulfuric acid-T solution for 24 h before use) in a 50-liter clean beaker. Add nitric acid solution (see 5.1.3.19) and dissolve it. Transfer the whole amount to a 109-ml volumetric flask. Add nitric acid solution (see 5.1.3.19) to make up to the mark. Mix well. 5.1.3.13 Prepare standard intermediate solution (10.1 g/ml): Take 0.0 g of HgCl. 1ml. Standard stock solution (see 5.1.3.12) is placed in a 190 ml volumetric flask. Add acid solution (see 5.1.3.10) to the mark: Mix 5.1.3.14 Mercury standard intermediate solution (0.100 μg/ml); Transfer 1.0 ml. Standard intermediate solution (see 5.1.3.3) is placed in a 109 ml volumetric flask. Add acid solution (see 5.1.3.1) to the mark and mix: 5.1.3.15 Mercury standard ready-to-use solution (10.0 ng/mL): Transfer 19.0 ml of standard solution (see 5.1.3.14) to a 100 ml volumetric flask. Add acid solution (see 5.1.3.10) to the mark: Mix: rml volumetric flask. Add nitric acid solution (see 5.1, 3.10) to the mark. Mix well (prepare before use). 5.1.4 Instruments and equipment
Instruments and equipment for fluorescence spectrophotometry are as follows:
Volumetric flask: capacity 100 ml., 1 900 ml.: - Pipette: capacity 1m2 m.
- Beaker: capacity 50 ml, 1 000 ml; ---- General laboratory instruments and equipment 5.1.5 Analysis steps
5.1.5.1 Draw a standard curve
5. 1. 5. 1. 1 Measure 0 ml., 0. 25 mL, C. 50 ml,, 1. GO mI., 2. G0 rmL, 4. 00 ml., 8. 90 ml. Calculate the standard solution (5.1.3.1) and transfer it to a 10 m volumetric flask. Add sulfuric acid solution (see 5.1.3.9) to the mark. Mix and add 2.0 ml of each sample. Determine the light intensity value of each point in the standard column according to the value of the light intensity of the standard blank (I) (5.15.1.2) and change (1) to the ordinate and calculate the H coefficient. Draw a standard curve (give the linear regression curve) and calculate the H coefficient. The result is recorded in Table A.1.
5.1.5.2 Sample determination
5.1.5.2.1 Sample digestion: Take 100 ml of water sample and put it into a 250 ml conical flask. Add 2.0 ml of sulfuric acid (see 5.1.3.1) and 5.0 ml of persulfate solution (see 1.3.8). Place it at room temperature for 24 h or boil it for 1 min. Cool it to room temperature. Add 2 ml. Hydroxylamine solution (see 5.1.3.7). Mix well. This solution is the sample digestion solution. 5.1.5.2.2 Analysis blank: Measure 100 ml. Pure water into 259 ml. Chain bottle, add 2.0 ml. Sulfuric acid (see 5.1.3.1). 5.0 ml potassium persulfate solution (see 5.1.3.8). Place it under room temperature to digest for more than 24 hours or heat and boil for 1 minute, then cool to room temperature: 3
GB17378.4—2007
Add 2 ml. Hydroxylamine hydrochloride solution (i.e. 5.［.3.7), mix - this solution is the analytical blank solution, 5.1.5.2.3 take 2.0mL of sample digestion solution (see 5.1.5.3, 1) and analytical blank solution (see 5.1.5.3.2) in the oxide generator, measure the blank fluorescence intensity (1) and the fluorescence intensity (1,) of the sample digestion solution. With the value of (1, -I), the required amount (g) can be obtained from the standard curve or the mercury amount can be calculated using the linear regression equation (). 5.1.6 Record and calculate
Record the sample measurement data in Table A.2. Calculate the required content in seawater according to formula (2): F
Where:
is the concentration of mercury in the water sample, in micrograms per liter (μg/l); m is the mercury content in the water sample, in nanograms (ng); m is the volume of the sample after digestion, and the positive coefficient is 1. Proof: V is the injection volume, in liters (ml.), 5.1.7 Precision and accuracy
When the concentration is 1.0) μg/l, the repeatability relative standard deviation is 2.5%; the reproducibility relative standard deviation is 10.2%; the relative error is 6.5%. 5.1.8 Precautions
The following precautions should be taken during the implementation of this method: Unless otherwise specified, all reagents used in this method are analytically pure. Water is mercury-free pure water or equivalent pure water.
|| All instruments used in the test must be soaked in nitric acid solution (1-3) for 24 hours and then rinsed with deionized water before use;
|| During the test, do not allow the instruments to be contaminated by the reagents
|| The content of hydroxylamine hydrochloride varies greatly. Before use, a reagent blank test should be performed to avoid excessive blanks and cause large measurement errors.
|| There are many factors that affect the determination of the reagents, such as carrier gas flow, mercury lamp current, negative voltage, etc. Therefore, each measurement should be measured in a standard series.
|| 5.2 Cold atomic absorption spectrophotometry
|| 5.2.1 Scope and application areas
|| Applicable to the determination of mercury in seawater in oceans, coastal areas and estuaries. 5.2.2 Principle of the method
The water sample is digested with sulfuric acid-potassium chloride. Under the action of reducing agent stannous chloride, the ions are reduced to mercury. The characteristic absorption value of mercury atoms is measured at 253.7TiI wavelength using a liquid balance open-circuit aspiration system. 5.2.3 Reagents and their preparation
52.3.1 Potassium sulfate (KS)
5.2.3.2 Calcium chloride (CHCl.); used to fill the drying tube 5.2.3.3 Low mercury seawater: Surface seawater is filtered through filter paper. The mercury content should be less than C.005u%/1-5.2.3.4 Nitric acid solution (1 +19): Slowly add 50 ml of nitric acid (g=1.42 g/nL) to 1 000l ml. water, 5.2.3.5 Sulfuric acid solution (1+1): add 1:1 sulfuric acid (-1.8z/mJ) slowly into 60ml. water 5.2.3.6 Sulfuric acid solution (0.5imo1/1): add 28ml. sulfuric acid (a--1.8g/ml) slowly into water under stirring and dilute to 1/1. 5.2.3.7 Hydrochloric acid solution (1+1): dilute hydrochloric acid (-1, [9 g/ml) with an equal volume of water. 5.2.3.8 Hydroxylamine hydrochloride solution (100 g/1): weigh 2 hydroxylamine hydrochloride (NI:0H·HCh) into water and dilute to 20 ml. 5.2.3.9 Stannous chloride solution: weigh [0.9 stannous chloride (Smt.)] into a beaker and add 0.1 ml. hydrochloric acid (see 5.2.3.7). Heat until stannous chloride is completely dissolved, cool and place in a reagent bottle: dilute with an equal volume of water before use: when the mercury impurity is high, add nitrogen to remove the mercury until the mercury content is undetectable.
GB 17378. 4--2007
5.2.3.10 Mercury standard preparation solution (1.00 mg/tnL Hg): weigh 0.135 4 mercuric chloride (HgCl. Pre-dried in a sulfuric acid desiccator) in a 10 ml beaker, dissolve it with nitric acid solution (see 5.2.3.1), transfer the whole amount to a 100 ml bottle, add nitric acid solution (see 5.2.3.4) to dilute to the mark, mix. Place in a brown borosilicate glass reagent bottle, the storage period of this solution is ~ years. 5.2.3.11 Multiply the standard intermediate solution (10.0 ug/m1.) Pipette 1.00 1L of the standard stock solution (see 5.2.3.10) into a 100 HIL volumetric flask, add nitric acid solution (see 5.2.3.4) to dilute to the mark, mix well, and this solution can be stored for one week. 5.2.3.12 Mercury standard solution (0.02 μg/ml/L): Pipette 1.00 ml of the intermediate solution of mercury standard (see 5.2.3.11) into a 100 mL flask, add sulfuric acid solution (see 5.2.3.6) to dilute to the mark, and mix. 5.2.4 Instruments and equipment The instruments and equipment are as follows: A mercury measuring device is shown in the figure. Mercury vapor generating bottle: made of a 250 mL conical glass washing bottle. Cut the lower end of the vent tube of the washing bottle so that the end of the tube just leaves the liquid surface to be measured. A volumetric flask: capacity 100 mL; A graduated pipette: capacity 0.2 mL, 0.5 mL, 1 mL, 2 mL, 5 InI.; A transfer pipette: capacity 1 ml. Reagent bottle: capacity 250 ml.,500 mI.1 000 mL, 250 ml.;—General laboratory instruments and equipment
1-Air pump:
2-Air flow regulating valve;
3-Exhaust gas absorber
4-Recorder;
: Light absorption cell:
6-Drying tube
7-Two-way valve:
8--Exhaust gas generating bottle;
9: Tight purification device;
10-Activated carbon absorber;
11-Gas flow meter.
Figure 1 Cold atomic absorption mercury measuring device
5.2.5 Analysis steps
5.2.5.1 Drawing a standard curve
5.2.5.1.1 Take 6 mercury vapor generating bottles and fill them with 100 ml low-temperature seawater (see 5.2.3.3) and 2.5 ml sulfuric acid solution (see 5.2.3.5), shake well, and use a 0.2 ml graduated pipette to transfer 0 ml.. 0.010 ml., 0.020 ml.. 0.040 ml., 0.0t0 ml..0.080 ml multiplied by the standard working solution (see 5.2.3.12), mix, 5.2.5.1.2 Turn the three-way switch (7) of the mercury measuring system_F to the zeroing position, and let air at a flow rate of 1 L/min~1.5 L/min pass through the light absorption cell
5. 2.5.1.3 Connect the mercury vapor generating bottle to the mercury measuring system in turn, add 2.0 ml of stannous chloride solution (see 5.2.3.9). Plug the bottle tightly for 5
GB 17378. 4-2007
, and shake vigorously for |min.
5.2.5.1.4: Adjust the zero point of the measuring instrument, turn the three-way switch to the measurement position, and measure its absorbance value 4.5.2.5.1.5 Record the data in Table 3. The absorbance value A: A, (standard narrow) is the vertical axis and the corresponding mercury amount () is the horizontal axis to draw a standard curve.
5.2.5.2 Water sample determination
5.2.5.2.1 Take 1:0-ml water sample and put it into a 25-ml hoop bottle, add 2.5 ml sulfuric acid solution (see 5.2.3.5), 0.25 g potassium persulfate (see 2.3.1) and place it at room temperature to digest for more than 10 minutes, or heat and boil for 1 minute and then cool to room temperature (when sampling, you can also add the above two digestion agents according to the metered amount): add 2.mL hydroxylamine hydrochloride solution (see 2.3.8) dropwise. 5.2.5.2.2 Transfer the water sample to a non-steam generating bottle (pay attention to remove all chlorine gas 1) and determine its absorbance value Aw according to the steps of 5.2.5.1.2 to 5.2.5.1.4.
5.2.5.2.3 Take 1C0 mL of pure water, determine the analytical value A.c5 according to the above steps, 2.6 record and calculate
record the sample determination data in Table A, 1, mountain (A4, -A) value to check the standard curve to get the mercury content m, or use linear regression to calculate m4-. Calculate the concentration in the water sample according to formula (3): value: Zhang =
water sample concentration. The unit is microgram per liter 1): Table-determined sample volume calibration coefficient is 1.; mercury content in water sample-unit is microgram per liter (): V. 2 water sample volume, unit is liter (ml); 4--curve cutoff:
b~Pa line slope, bzxZ.net
5.2.7 precision and accuracy
concentration is 1.251/1. When the relative error is 0.50%, repeatability (r) is 0.17μg/1. Repeatability relative standard deviation is 4.8; reproducibility (R) is 0.37ug/1. The relative standard deviation is 9.3%5,2.8. Precautions
Pay attention to the following items when implementing this method: Unless otherwise specified, all reagents used in this method are analytically pure. Water is mercury-free pure water or equivalent pure water: mercury ions are extremely unstable in distilled water, so the standard series should be prepared with filtered seawater or 2% sodium chloride solution;
--Chlorine affects the measurement results. Before the measurement, the gas in the digestion sample must be removed, otherwise the result will be too high; all instruments used must be soaked in nitric acid solution (i3}1 d. Check the table: the used mercury vapor generating bottle must be washed with acidic manganese acid lacquer solution and then rinsed with water. 5.3 Gold trap cold atomic absorption spectrophotometry
5.3.1 Scope and application field
Determination of mercury in ocean water, swimming water, surface water, etc. 5.3.2 Principle of the method
The sample is digested with sulfuric acid-potassium persulfate, and organic mercury is converted into inorganic mercury. Under the action of the reducing agent stannous chloride, mercury is reduced to metallic mercury. Mercury vapor is carried into the gold trap by the carrier gas and is combined with the gold wire to form gold. Heat the gold wire: release the mercury vapor, which is introduced into the absorption cell of the measuring instrument with the carrier gas. It is measured at 23.7nm. The characteristic absorption value of the mercury atom is 64: Adjust the zero point of the measuring instrument, turn the three-way switch to the determination gear, and measure its absorbance value 4.5.2.5.1.5. Record the data in Table 3. The absorbance value A: A, (standard narrow) is the vertical axis and the corresponding amount of mercury () is the horizontal axis to draw a standard curve.
5.2.5.2 Water sample determination
5.2.5.2.1 Take 1:0)-ml water sample and put it in 25l ml hoop bottle, add 2.5 ml sulfuric acid solution (see 5.2.3.5), 0.25 g potassium persulfate (see!.2.3,1) and place it at room temperature to digest Hn or more, or heat and boil for! min and then cool to room temperature (when sampling, you can also add the above two digestion agents according to the metered amount): add 2.mL hydroxylamine hydrochloride solution (see, 2.3.8). 5.2.5.2.2 Transfer the water sample to a non-steam generating bottle (make sure to remove all chlorine 1). For the rest, follow the steps in 5.2.5.1.2 to 5.2.5.1.4 to determine the absorbance value Aw
5.2. 5.2.3 Measure 1C0 mL of pure water, determine the analytical value A.c5 according to the above steps, 2.6 record and calculate
record the sample determination data in Table A, 1, mountain (A4, -A) value to check the standard curve to get the mercury content m, or use linear regression to calculate m4-. Calculate the concentration in the water sample according to formula (3): value: Zhang =
water sample concentration. The unit is microgram per liter 1): Table-determined sample volume calibration coefficient is 1.; mercury content in water sample-unit is microgram per liter (): V. 2 water sample volume, unit is liter (ml); 4--curve cutoff:
b~Pa line slope,
5.2.7 precision and accuracy
concentration is 1.251/1. When the relative error is 0.50%, repeatability (r) is 0.17μg/1. Repeatability relative standard deviation is 4.8; reproducibility (R) is 0.37ug/1. The relative standard deviation is 9.3%5,2.8. Precautions
Pay attention to the following items when implementing this method: Unless otherwise specified, all reagents used in this method are analytically pure. Water is mercury-free pure water or equivalent pure water: mercury ions are extremely unstable in distilled water, so the standard series should be prepared with filtered seawater or 2% sodium chloride solution;
--Chlorine affects the measurement results. Before the measurement, the gas in the digestion sample must be removed, otherwise the result will be too high; all instruments used must be soaked in nitric acid solution (i3}1 d. Check the table: the used mercury vapor generating bottle must be washed with acidic manganese acid lacquer solution and then rinsed with water. 5.3 Gold trap cold atomic absorption spectrophotometry
5.3.1 Scope and application field
Determination of mercury in ocean water, swimming water, surface water, etc. 5.3.2 Principle of the method
The sample is digested with sulfuric acid-potassium persulfate, and organic mercury is converted into inorganic mercury. Under the action of the reducing agent stannous chloride, mercury is reduced to metallic mercury. Mercury vapor is carried into the gold trap by the carrier gas and is combined with the gold wire to form gold. Heat the gold wire: release the mercury vapor, which is introduced into the absorption cell of the measuring instrument with the carrier gas. It is measured at 23.7nm. The characteristic absorption value of the mercury atom is 64: Adjust the zero point of the measuring instrument, turn the three-way switch to the determination gear, and measure its absorbance value 4.5.2.5.1.5. Record the data in Table 3. The absorbance value A: A, (standard narrow) is the vertical axis and the corresponding amount of mercury () is the horizontal axis to draw a standard curve.
5.2.5.2 Water sample determination
5.2.5.2.1 Take 1:0)-ml water sample and put it in 25l ml hoop bottle, add 2.5 ml sulfuric acid solution (see 5.2.3.5), 0.25 g potassium persulfate (see!.2.3,1) and place it at room temperature to digest Hn or more, or heat and boil for! min and then cool to room temperature (when sampling, you can also add the above two digestion agents according to the metered amount): add 2.mL hydroxylamine hydrochloride solution (see, 2.3.8). 5.2.5.2.2 Transfer the water sample to a non-steam generating bottle (make sure to remove all chlorine 1). For the rest, follow the steps in 5.2.5.1.2 to 5.2.5.1.4 to determine the absorbance value Aw
5.2. 5.2.3 Measure 1C0 mL of pure water, determine the analytical value A.c5 according to the above steps, 2.6 record and calculate
record the sample determination data in Table A, 1, mountain (A4, -A) value to check the standard curve to get the mercury content m, or use linear regression to calculate m4-. Calculate the concentration in the water sample according to formula (3): value: Zhang =
water sample concentration. The unit is microgram per liter 1): Table-determined sample volume calibration coefficient is 1.; mercury content in water sample-unit is microgram per liter (): V. 2 water sample volume, unit is liter (ml); 4--curve cutoff:
b~Pa line slope,
5.2.7 precision and accuracy
concentration is 1.251/1. When the relative error is 0.50%, repeatability (r) is 0.17μg/1. Repeatability relative standard deviation is 4.8; reproducibility (R) is 0.37ug/1. The relative standard deviation is 9.3%5,2.8. Precautions
Pay attention to the following items when implementing this method: Unless otherwise specified, all reagents used in this method are analytically pure. Water is mercury-free pure water or equivalent pure water: mercury ions are extremely unstable in distilled water, so the standard series should be prepared with filtered seawater or 2% sodium chloride solution;
--Chlorine affects the measurement results. Before the measurement, the gas in the digestion sample must be removed, otherwise the result will be too high; all instruments used must be soaked in nitric acid solution (i3}1 d. Check the table: the used mercury vapor generating bottle must be washed with acidic manganese acid lacquer solution and then rinsed with water. 5.3 Gold trap cold atomic absorption spectrophotometry
5.3.1 Scope and application field
Determination of mercury in ocean water, swimming water, surface water, etc. 5.3.2 Principle of the method
The sample is digested with sulfuric acid-potassium persulfate, and organic mercury is converted into inorganic mercury. Under the action of the reducing agent stannous chloride, mercury is reduced to metallic mercury. Mercury vapor is carried into the gold trap by the carrier gas and is combined with the gold wire to form gold. Heat the gold wire: release the mercury vapor, which is introduced into the absorption cell of the measuring instrument with the carrier gas. It is measured at 23.7nm. The characteristic absorption value of the mercury atom is 6
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