This standard provides 65 analytical methods for 33 seawater measurement items, and provides technical regulations and requirements for the sample collection, storage, transportation, and calculation of measurement results of seawater analysis. This standard is applicable to the areas of mixed freshwater and salty water in the ocean, offshore, and estuaries with different pollution levels. It can be used for marine environmental monitoring, routine water quality monitoring, environmental pollution investigation and monitoring in nearshore shallow waters (within the 0~5m isobath), 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 17378.4-1998 Marine Monitoring Specification Part 4: Seawater Analysis GB17378.4-1998 Standard Download Decompression Password: www.bzxz.net
This standard provides 65 analytical methods for 33 seawater measurement items, and provides technical regulations and requirements for the sample collection, storage, transportation, and calculation of measurement results of seawater analysis. This standard is applicable to the areas of varying degrees of pollution in the ocean, offshore, and estuaries, as well as mixed fresh and brackish water. It can be used for marine environmental monitoring, routine water quality monitoring, environmental pollution investigation and monitoring in shallow coastal waters (within the 0-5m isobath), 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 17378.4-1998
This standard is the fourth part of the "Ocean Monitoring Specifications", which is revised on the basis of the HY 003.4-1991 industry standard. This standard is the technical regulations and requirements for seawater analysis. The National Marine Monitoring Specifications include the following parts: GR 17378.1-1998 Marine Monitoring Specifications Part 1 General Principles GI 17378. 2—1998 GB 17378.3—1998 GB 17378-4—1998 Marine Monitoring Specifications Part 2: Data Processing and Analysis Quality Control Marine Monitoring Specifications Part 3: Sample Collection, Storage and Transportation Marine Monitoring Specifications Part 4 Seawater Analysis Part 5 Sediment Analysis GB 17378. 5—1998 Marine Monitoring Specifications Part 6: Biomass Analysis GB 17378. 6—1998
Part 7, Ecological survey and biological monitoring of offshore pollution GB 17378. 7---1998
: Marine monitoring specifications
Appendix A and Appendix B of this standard are both appendices of the standard. This standard is proposed by the State Oceanic Administration. Www.bzxZ.net
This standard is under the jurisdiction of the National Marine Standards and Metrology Center. This standard is drafted by the National Marine Environmental Monitoring Center, and the main drafters of this standard are Zhang Chunming, Xu Kuncan, Chen Weiyue, Chen Banglong, Zhan Xiuwen, and Xu Zhen. 1 Scope
National Standard of the People's Republic of China
Specification for marine monitoring Part 4: Seawater analysis
The specificatin for marine monitoring Part d: Seawater tnalysis
GB 17378. 4 1998
This standard provides 65 analytical methods for 33 seawater measurement items, and provides technical regulations and requirements for sample collection, storage, transportation, and calculation of measurement results of seawater analysis.
This standard is applicable to the pollution level of oceans, offshore, ports and estuaries, and the mixed water of Weidan. It can be used for marine environmental monitoring, routine water quality monitoring, environmental pollution investigation and monitoring of nearshore shallow waters (within the 0-5m isobath), 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. 2 Referenced standards
The provisions contained in the following standards are constituted as the provisions of this standard by reference in this standard. At the time of publication of this standard, the versions shown are valid. All standards are subject to revision, and parties using this standard should discuss the possibility of using the latest versions of the following standards GB12763.2-91, Marine Survey Specification Marine Hydrological Observation GB12763.4-91 Marine Survey Specification Marine Chemical Element Observation GB17378.3-1998 Marine Monitoring Specification Sample Collection, Storage and Transportation GB1737B.2-1998 Marine Monitoring Specification Data Processing and Analysis Quality Control ZBY116-82 Inverted Temperature Table
3 Definitions
This standard adopts the following definitions.
3.1 Filterable (sobuble) metals Filterable (sobuble) metals Metal components in unacidified water samples that can pass through a 0.45um filter membrane. 3.2 Unfilterable (suspended) metals Unfilterable (suspcnded) metals Metal components in unacidified water samples that are retained by a 0.45μm filter membrane. 3.3 Total metals
The sum of filterable metals and unfiltered gold in water sample. 3.4 Acid extractable metals The gold content of unfiltered water sample after treatment with hot dilute inorganic acid. 3.5 Filtered water sample Filtered water &le Unless otherwise specified, refers to water filtered with a 0.45μm fiber filter membrane. Approved by the State Administration of Quality and Technical Supervision on June 22, 1998 and implemented on January 1, 1999
4 General provisions
4.1 Purification and treatment of reagents, solvents and filter membranes GB 17378. 4-1998
4.1.1 Purification of ammonia water by isothermal diffusion method: Place containers containing ammonia water and high-purity water on or under the partition of the glass desiccator and place them in a sealed manner. The diffusion time depends on the temperature, about 1 to 2. 4.1.2 Purification and preparation of disulfide: see 6.2.3.7. 4.1.3 Purification of trichloromethane and carbon tetrachloride: A simple treatment can be performed on the newly opened agent, that is, add 200mL of hydroxylamine hydrochloride solution (0.5%) to each liter of solvent in the separatory colander to wash and discard the water phase, then wash once with pure water, and filter through dried filter paper. If it is a recycled waste agent or one that is still unqualified after the above treatment, use the following method instead: Pour the solvent into the distillation bottle until it is half full, cover the upper layer with an appropriate amount of sodium sulfite solution (10%), perform the first distillation, then transfer it to another clean distillation bottle, add solid calcium oxide for the second distillation, discard a little of the initial filling liquid, collect the distillate, and put it in a brown bottle. If the solvent is chlorinated pseudoephedrine, 1% volume of anhydrous ethanol can be added to increase its stability.
4.1.4 Treatment of 0.45um fiber filter membrane: Hold the edge of the filter membrane with a stainless steel tube covered with polyethylene film, and immerse each filter vertically downward in a 0.5mol/1. hydrochloric acid solution for at least 12 hours. Rinse with pure water until neutral, seal and set aside. 4.2 Notes
4.2.1 Subtraction of standard blank (A) and analytical blank (Ab>4.2.1.1 When A.=A (i.e. the determination steps of the standard series and the water sample are completely consistent), both do not need to be subtracted, i.e. A is not subtracted from A. Draw a calibration curve or read the curve, but it is only feasible for the same batch: If the blank value (A. and A) is very stable, it can be used for: weeks. Absorbance (signal) value of ice sample:
Ab: absorbance value of analytical blank;
A: absorbance value of each point in the standard series, where zero degree is the standard blank A.. 4.2.1.2 When A. . ≠Ab, that is, when the determination steps of the standard series are omitted compared to the water sample, then A, -A. must be used to draw the curve; A, A. must be used to read the curve.
4.2.1-3 Calculations using linear regression equations should also follow the above provisions. 4.2.1.4 Determination methods such as atomic absorption, gas chromatography electrochemistry, etc., refer to the above provisions. 4-2.2 Correction of salt error
In order to reduce salt error (error caused by different ion strengths), some projects require the use of clean seawater to dilute the standard series. If pure water is used, a correction factor must be given. It is known that some correction factors (such as silicon, Ammonia) is greatly affected by the environment and pure water, so the user must make necessary corrections based on the actual measured results.
4-2.3 Correction of water sample volume
When the reagent solution added to the water sample exceeds 1% of the volume before measuring the water sample, perform volume correction according to formula (1): VV
V=V+Va
Where: - the volume of the water sample after correction, mL, Vi - the original water sample volume, mL
V2 - the volume of the added reagent solution, mL;
V, the volume of the water sample measured, ml.
4.2 .4 Test methods for water temperature, salinity, water color, transparency, pH, etc. +++++*er(I)
4.2.5 Test methods for nitrogen compounds, chemical oxygen content, ammonia bromate method, etc. are equivalent to classical methods at home and abroad. Most of their performance indicators are quoted from the original manuscript and have not been verified.
42.6 Repeated determination of relative deviation limits between parallel samples and natural sample spike recovery rates. If not specified in the original method, follow the provisions of GB17378.2-1998.
4.3 Water sample collection, storage and transportation
GB17378. 41998
The determination of the sampling position of seawater samples and the selection of the time and space frequency, sampling equipment, sampling equipment and other basic equipment, the storage and preservation of sampling bottles, and the requirements for on-site sampling operations, storage and transportation of samples are detailed in GB17378.3. The water sample volume and preservation method required for each test item and its analysis method are listed in Table 1. Table 1 Water sample volume and preservation method
Test items and methods
Cold atomic absorption
Spectrophotometry
Disulfide spectrophotometry
Spectrophotometry
Gold atom
Atom absorption
Flameless atomic
Absorption spectroscopy
7.2. Anodic stripping voltammetry, flame-baked atomic absorption spectrophotometry, di-N-ammonia dithiocarbamate spectrophotometry, no flame atom, absorption spectrophotometry, anodic stripping voltammetry, flame atomic absorption spectrophotometry, dithiol spectrophotometry, sampler material, plastic or glass, glass or plastic, water ladder on-site pretreatment, add H2SO4 until, add HSO4, To
add H.SO.To
add HsO,To
filter and add HNOa
to pH2
filter as HNO;
to pH2
over discharge add HND
to pH2
filter and add HNK):
to pH2
over discharge add HNO,
to pH2
filter and add HNO,
Pen pH2
Filter and add HNO:
To pH2
Filter and add HNO,
To pH≤2
Filter and add HNU,
To pH≤2
Filter and add HNO.
To pH<2
Water sample dosage
Stored container
Recommended temperature
Overflow: refers to
0. 45 μm Sugar film P: B-plastic G: Hard glass. The water sample is analyzed once with a plate. The sample volume used for the analysis should be multiplied by the number of repeated measurements. The following measurement items and methods include flame atomic absorption spectrophotometry and extreme dissolution atomic absorption spectrophotometry. Dithiol spectrophotometry. Flame atomic absorption spectrophotometry. 1G.3 Double tracking spectrophotometry Diphenylcarbazide spectrophotometry Non-fire atomic absorption spectrophotometry 12.1 Arsenic-nitric acid spectrophotometry Hydride generation ion absorption spectrophotometry Catalytic polarography Material of the sampler used Glass or plastic Glass or plastic Glass or material Glass or plastic GB 17378: 4—1998
Table 1 (continued)
On-site anodizing of ice samples
Add HNO
Water with water
Filter and add HNC
Filter and add JINO
Filter and add HNO
To pH 2
Filter as HNO;
To pH 2
Add HNO
Filter and add HN
Too thin and add HNO:
Filter and add HVO:
|To pH≤.2
Filter and add H.SO
Filter and add H,SO.
To pH2
Filter and add H,SO,
To pH<2
Filter and add H.SO
To pH2
Test container
Storage temperatureStorage
Three months
Testing method
Fluorescence spectrophotometry
Diazopylen
Amine spectrophotometry
13. 3|Catalytic polarography
Cyclohexane extraction
Fluorescence spectrometry
Cyclohexane system fluorescence
Spectrophotometry
Gravimetric method
Ultraviolet spectrometry
Gas chromatography
Polyoxybiphenyls
Gas chromatography
Dieldrin
Gas chromatography
Active silicate
Silica platinum yellow method
Silica molybdenum blue method
Sulfide| |tt||Methylene sulfone
Spectrophotometry
19.2 Ion-selective electrophoresis
Volatile phenol
4-nitroantipyrine
Spectrophotometry
The sampling equipment used is
glass or plastic
glass or gold
glass or metal
glass or gold
glass or metal
GB 17378. 4—1998
Table 1 (line)
Pretreatment of water samples on site
Filter and add HNO,
to pH 2
Extraction on site
Extraction on site
Extraction on site
Add
1 ml of zinc sulfate
solution (50R/1)
<4.
2 g of copper sulfate
(CuSO. +H)
Water sample dosage
10--200
Storage container
Storage temperature
Three months
Test items and methods
Cyanide
Isonicotinic acid-azole
Clear method
Indole-barbituric acid
Acid spectrophotometer
Material of sampler used
Glass or gold
Anion washing gold filter or glass
Toluene blue spectrophotometry
Ga and beads
Sensory method
PH meter method| |tt||pH colorimetric method
suspended matter
gravimetric method
chloride
gum titration method
salinity meter method
turbidity
nephelometry method
spectrophotometry
meltometer method
dissolution
32.1 iodine titration method
glass, plastic or metal
glass, plastic or metal
glass, plastic or metal
glass or metal
CB 17378. 41998
Table (continued)
Water-mixed on-site pretreatment
Add NaOH
PHE2~13
On-site filtration
Add 1 mL MnCl
and 1 mL iodine
Water sample quantity
Storage container
Storage humidity
On-site immediate determination
On-site immediate determination
Storable
Measurement items and methods
Chemical ammonia demand
33. 1Alkaline high-amplitude acid
Biochemical oxygen demand
Five-H culture method
Two-day culture method
(BOL)
Material of sampler used
Glass or metal
Glass or metal
Total organic carbon
Glass or metal
Potassium persulfate
Inorganic carbon
GB1737B.4—1998
Table 1 (end)
On-site pretreatment of water samples
Glass, filler or metal:
Phenol blue spectrophotometry
Photometric method||tt ||Substantial Oxygen
Nitrite
Ethylenediamine Spectrophotometry
Nitrate
Column Reduction Method
(Note)
Inorganic Phosphorus
Phosphomonblyl Blue Spectrophotometry
36.2 Phosphomolybdenum Blue-Extraction
Spectrophotometry
Glass, Plastic or Gold Layer
Drum Assisted, Plastic or Metal
Glass, Plastic or Metal Filter
Water Sample Volume
Note: The zinc method is equivalent to this method, see B12763.4-91 for details. Storage Container
Operating Temperature
Can be stored in a freezer for 48 h
See 31.1.5,7
If frozen at 20°C, it can be stored for 7 days
If it cannot be determined immediately
it should be stored in the refrigerator, but the detection limit cannot exceed
5
The detection limit (XN) of each method is listed in Table 2. Table 2 List of detection limits (XN) (reference values) of seawater analysis methods No.
Cold atomic absorption spectrophotometry
Double trace spectrophotometry
Gold trace cold absorption spectrophotometry
Measurement items and analysis methods
Flameless atomic absorption spectrophotometry
Anodic stripping voltammetry
Flame atomic absorption spectrophotometry
Sodium dinitrogen monocarboxylate spectrophotometry
.Flameless atomic absorption spectrophotometry
Anodic stripping voltammetry
Decomposition atomic absorption spectrophotometry
Dithiol spectrophotometry
Flameless atomic absorption spectrophotometry
Yang Gai Rong Chuan method
Fire-baked atomic absorption spectrophotometry|| tt||Dithiol spectrophotometry
Northern flame atomic absorption spectrophotometry
Anodic stripping voltammetry
Dithiol spectrophotometry
.Total complex
Diphenylcarbazide spectrophotometry
Flameless atomic absorption spectrophotometry
Arsine-silver nitrate spectrophotometry
Hydride generation atomic absorption spectrophotometry Guangguanghu method catalytic polarography
fluorescence spectrophotometry
diaminobiphenyl spectrophotometry
catalytic polarography
cyclohexane extraction fluorescence spectrophotometry
fluorine-cyclohexane system fluorescence spectrophotometry gravimetric method
ultraviolet spectrophotometry
gas chromatography
polybiphenyl
2. 7×1G 3
2. 0×102
Gas chromatography
Dieldrin
Gas chromatography
Active silicate
Silicon molybdenum yellow method
Molybdenum blue method
Vitriol
Methylene blue spectrophotometry
Ion selective electrode method
Volatile vanadium
GB 17378. 41998
Table 2 (continued)
Test items and analytical methods
4-aminoantipyrine spectrophotometry
Cyanide
isonicotinic acid-pyrazolone spectrophotometry
pyridine-barbituric acid spectrophotometry
Colorimetric
Transparency
Visual method
Anionic detergent
Methyl blue spectrophotometry
Taste
Sensory method
Water temperature measurement
Inverted thermometer method
pH Colorimetric method
Suspended matter
Gravimetric method
Oxide
Argentometric titration method
Saltometer
Turbidity
Oral spectrophotometry
Alkalimeter
Biochemical oxygen demand
Iodine method
Chemical demand
Potassium sulfate method
Biochemical oxygen demand
May culture method (R():)
Two-H culture method (BOD,)
Total organic carbon
Persulfate oxidation method
Inorganic nitrogen
Longpan blue spectrophotometry
Oxybromate oxidation method
Nitrite
Ethylenediamine spectrophotometry
Nitrate
Taowang reduction method
Zinc-Hydrogen reduction method
Inorganic hardness
Phosphate spectrophotometry
Phosphomolybdenum blue extraction spectrophotometry
Sulfide is expressed as S'.
2 Cyanide is represented by CN
6.1 Cold atomic absorption spectrophotometry
6.1.1 Scope and application fields
GB 17378. 4 1998
Table 2 (end)
Measurement items and analysis methods
Applicable to the determination of mercury in seawater in ocean, coastal and estuary areas. Detection limit: 1.0×10-g/L
6.1.2 Principle of the method
XN,uR/L
The water sample is digested with sulfuric acid and potassium persulfate. Under the action of the reducing agent stannous chloride, the mercury ions are reduced to metallic mercury. The characteristic absorption value of mercury atoms is determined at a wavelength of 253.7nm using a gas-liquid equilibrium open-circuit aspiration system. 6.1.3 Reagents and their preparation
Unless otherwise specified, all reagents used in this method are analytically pure, and water is mercury-free pure water or equivalent pure water. 6.1.3.1 Potassium persulfate (K,S0)
6.1.3.2 Anhydrous calcium fluoride (CaCl,): used to fill the drying tube. 6.73.3 Low-water seawater: The mercury content of surface seawater should be less than 0.0051 g/L after filtering with filter paper. 6.1.3.4 Nitric acid solution: 1+19
Dissolve 50ml nitric acid (p=1.42g/mL) with water to 1000ml.6.1.3.5 Sulfuric acid solution: 1+1
Add 500ml sulfuric acid (p=1.84g/mL) slowly to 500ml water under stirring.6.1.3.6 Sulfuric acid solution: 0.5mol/L
Add 28ml sulfuric acid (p1.84g/mL) slowly to water under stirring and dilute to 1L.6.1.3.7 Hydrochloric acid solution: 1+1
Dilute hydrochloric acid (μ=1.19g/mL) with an equal volume of water.6.1.3.8 Hydroxylamine hydrochloride solution: 100%/L
Weigh 25g hydroxylamine hydrochloride (NHzOH·HCI) in water and dilute to 250ml. 6.1.3.9 Stannous chloride solution
Weigh 100g of stannous chloride (SnCl2) into a beaker, add 500mL of hydrochloric acid solution (6.1.3.7), heat until the stannous chloride is completely dissolved, cool and place in a reagent bottle. Add an equal volume of water to dilute before use. When the mercury impurity is high, pass ammonia nitrogen gas to remove mercury until the mercury content is undetectable. 6-1.3.10 Standard preparation solution of mercury: 1.00mg/tnlHg. Weigh 0.1354% fluorinated hydride (HgCl2, dried in a sulfuric acid dryer in advance) into a 10ml beaker, dissolve it with nitric acid solution (6.1.3.4), transfer the entire amount into a 100mL volumetric flask, add nitric acid solution (6.1.3.1) to the mark, and mix. Stored in brown borosilicate glass reagent bottle, 1.00mL of this solution contains 1.00mg of mercury, and the shelf life is one year. 6.1.3.11 Mercury standard intermediate solution: 1h.0g/mL Pipette 1.03mL of mercury standard stock solution (6.1.3.12) into a 100L volumetric flask, add nitric acid solution (6.1.3.4) to dilute to the mark, and mix well. 1.00mL of this solution contains 10.0mg of mercury, and the shelf life is one week. 6.1.3.12 Mercury standard working solution, 0.100μg/ml, Pipette 1.00rnL of mercury standard intermediate solution (6.1-3.11) into a 100ml volumetric flask. Add sulfuric acid solution (6.1.8.6) to dilute to the mark, and mix well. 1.00mL of this solution contains 0.100g of mercury. Prepare. 6.1.4 Instruments and equipment
-See Figure 1 for the measuring device.
1—Vacuum pump: 2—Air flow regulating valve, 3—Containing waste gas absorber; 4—Measurement instrument; 5—Light absorption cell 16—Drying tube: 7—Three-way valve: 8—Mercury vapor generating bottle; 9—Air purification device: 10—Activated carbon absorber: 11—Gas flowmeter Figure 1 Cold atomic absorption measurement device
A mercury vapor generating bottle: modified from a 250mL conical glass washing bottle, the washing bottle ventilation tube is cut down so that the end of the tube just leaves the liquid surface to be measured;
—-Volume flask: 100ml;
—Graduated pipette: 0.20.5, 1.2, 5nL; a pipette: 1 ml.
—Reagent bottle: 250.500, 1000mL, brown 250ml.—A conical flask: 250mL;
General laboratory standing instruments and equipment.
6. 1.5 Analysis steps
6.1.5.1 Draw a standard curve
6.1.5.1.1 Take 6 mercury vapor generating bottles, add 100ml of low mercury seawater (6.1.3.3) and 2.5mL of sulfuric acid solution (6.1.3.5) respectively. Mix well, and use a 0.2ml graduated pipette to transfer 0, 0.010, 0.02, 0.040, 0.060, and 0.080ml of standard working solution (6.1.3.12) respectively, and mix well
6.1.5.1.2 Turn the three-way switch (7) on the mercury measuring system to the zeroing position: pass air through the light absorption cell at a flow rate of 1 to 1.5 L/min. 6.1.5.1.3 Connect the mercury vapor generating bottles to the mercury measuring system in turn, add 2.0 mL of stannous chloride solution (6.1.3.9), plug the bottle stopper, and shake vigorously for 1 min.
6.1.5.1.4 Adjust the zero point of the mercury analyzer. Turn the three-way switch to the determination position. Measure its absorbance value A. 6.1.5.1.5 Record the data in Appendix Table A1, with the absorbance value A, -A standard blank) as the ordinate and the corresponding mercury disk (yield g) as the abscissa, and draw a standard curve.
6.1.5.2 Water sample determination
6.1.5.2.1 Collect 100 ml of water sample in a 250 mL conical flask, add 2.5 ml of vegetable acid solution (6.1.3.5) and 0.25 more potassium persulfate
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