GB 15581-1995 Caustic soda and polyvinyl chloride industrial water pollutant discharge standards
Some standard content:
National Standard of the People's Republic of China
Discharge standard of water pollutants forcaustic alkali and polyvinyl chloride industryGB15581-95
3.8978-88
replaces GB
Caustic soda part
In order to implement the "Environmental Protection Law of the People's Republic of China", "Water Pollution Prevention and Control Law of the People's Republic of China", and "Marine Environmental Protection Law of the People's Republic of China", promote caustic soda, polyvinyl chloride This standard is specially developed to prevent and control water pollution due to advances in industrial production processes and pollution control technologies. 1 Subject content and scope of application
1.1 Subject content
This standard stipulates the maximum allowable discharge concentration of caustic soda and polyvinyl chloride industrial water pollutants and the maximum per ton product per year according to the production process and wastewater discharge destination. Drainage allowed.
1.2 Scope of application
This standard is applicable to the caustic soda and polyvinyl chloride industries (including the production of liquid alkali, solid alkali and Hydrochloride treatment process, as well as the emission management of polyvinyl chloride and other products using hydrogen, chlorine, ethylene, calcium carbide as raw materials) enterprises, as well as the environmental impact assessment, design, completion acceptance and post-completion emission management of construction projects. This standard does not apply to caustic soda.
2 cited standards
GB3097
Sea water quality standard
GB3838 Surface water environmental quality standard
GB6920 Determination of water quality pH value by glass electrode method GB7468 water quality| |tt||Determination of total mercury by cold atomic absorption spectrophotometry GB7469
Water quality
Determination of total mercury by potassium permanganate-potassium persulfate digestion method by disulfide spectrophotometry GB7488||tt ||Measurement of five-day biochemical oxygen demand (BOD,) by dilution and inoculation method for water quality
GR8978
GB11897
GB11898
GB11901
Sewage comprehensive Emission standards
Determination of free chlorine and total chlorine in water quality N,N-diethyl-1,4-phenylenediamine titration method Water quality
Determination of free nitrogen and total chlorine N,N-diamine .Ethyl-1,4-phenylenediamine spectrophotometry Water quality
Determination of suspended solids Gravimetric method
GB11914 Water quality Determination of chemical oxygen demand Dichromate method 3 terms||tt| |3.1 Caustic soda industrial wastewater
refers to the wastewater discharged from the treatment process of producing liquid alkali, solid alkali and hydrogen chloride using salt water as raw material using mercury electrolysis, diaphragm electrolysis and ion exchange membrane electrolysis.
3.1.1 Mercury electrolysis
refers to the production process of using salt water as raw material and using mercury electrolytic cells to produce liquid alkali, solid alkali and hydrogen chloride treatment process approved by the National Environmental Protection Bureau on June 12, 1995 1996-07-01 Implementation
: com3.1.2 Diaphragm Electrolysis Method
GB15581-95
refers to the production of liquid alkali, solid alkali and hydrogen chloride using diaphragm electrolytic cells with salt water as raw material The production process of the treatment process, wastewater includes net water, chlorine-containing wastewater and alkali-containing wastewater.
3.1.2.1 Net water
The net water referred to in this standard is the cleaning water of the diaphragm electrolytic cell and the flushing and drainage of the tank repair. 3.1.3 Ion exchange membrane electrolysis
refers to the production process of using salt water as raw material and using ion exchange membrane electrolyzer to produce liquid alkali, solid alkali and chlorine hydrogen treatment process. Wastewater includes chlorine-containing wastewater and alkali-containing wastewater.
3.2 Polyvinyl chloride industrial wastewater
refers to the wastewater discharged during the production process of polyvinyl chloride using chlorine, hydrogen, ethylene and calcium carbide as raw materials. 3.2.1 Calcium carbide method
refers to the production process of producing polyvinyl chloride using calcium carbide, chlorine and hydrogen as raw materials. The wastewater includes calcium carbide wastewater and PVC wastewater. 3.2.1.1 Calcium carbide wastewater
refers to the carbide slag slurry (liquid) and wastewater discharged from the process of producing vinyl chloride monomer using calcium carbide as raw material. 3.2.2 Ethylene oxychlorination method
refers to the production process of polyvinyl chloride using ethylene oxychlorination method using chlorine, ethylene and oxygen as raw materials. 4 Technical Internal Customers
4.1 Enterprise Types
According to product processing categories, they are divided into: caustic soda enterprises and polyvinyl chloride enterprises. 4.1.1 Caustic soda enterprises are divided according to production processes: mercury electrolysis, diaphragm electrolysis, and ion exchange membrane electrolysis. 4.1.2 Polyvinyl chloride enterprises are divided according to production processes: calcium carbide method PVC, ethylene oxychlorination method PVC. 4.2 Standard classification
The standard classification is divided according to the type of discharge into the water area. 4.2.1 Wastewater discharged into Class II waters in GB3838 (except water body protection areas) and Class III sea areas in GB3097 shall be subject to the first-level standards. 4.2.2 Wastewater discharged into Category V and V waters in GB3838 and Category IV sea areas in GB3097 shall be subject to secondary standards. 4.2.3 Wastewater discharged into the urban sewer network with a secondary sewage treatment plant shall comply with the third-level standard. 4.2.4 Wastewater discharged into urban sewer pipe networks without secondary sewage treatment plants must comply with the provisions of 4.2.1 and 4.2.2 respectively based on the functional requirements of the sewer effluent receiving waters. 4.2.5 In Class 1 and Class I waters and water body protection zones in Class 1 waters in GB3838, and Class II sea areas in GB3097, new sewage outlets are prohibited, and expansion and reconstruction projects are not allowed to increase the amount of sewage discharge. 4.3 Standard value
This standard stipulates the maximum allowable emission concentration of caustic soda and polyvinyl fluoride industrial water pollutants and the maximum allowable drainage volume per ton of product according to different years.
4.3.1 Caustic soda enterprises constructed before January 1, 1989 shall comply with Table 1, and polyvinyl chloride enterprises shall comply with Table 2. 4.3.2 Caustic soda enterprises constructed between January 1, 1989 and June 30, 1996 shall comply with Table 3, and polyvinyl chloride enterprises shall comply with Table 4.
4.3.3 Caustic soda enterprises constructed since July 1, 1996 shall comply with Table 5, and vinyl chloride enterprises shall comply with Table 6. 4.3.4 The standard implementation years shall be determined according to the approval date of the enterprise environmental impact assessment report (table) of the construction company in accordance with the provisions of Articles 4.3.1, 4.3.2 and 4.3.3 respectively; for construction without the approval of the environmental protection administrative department Enterprises should determine the implementation period of the standard based on the approval date of the supplementary environmental impact report (form). 4.4 Other regulations
4.4.1 Salt mud water is not allowed to be discharged into caustic soda wastewater. : comGB15581—95
4.4.2 The maximum allowable emission concentration of pollutants is calculated based on the daily average, and the maximum allowable discharge per ton of product is calculated based on the monthly average. The maximum allowable drainage volume per ton of product does not include indirect cooling water, domestic sewage in the factory area, and drainage from boilers and power stations in the factory. 4.4.3 If caustic soda and polyvinyl chloride enterprises discharge mixed wastewater that is not a single product, or caustic soda and polyvinyl chloride industrial wastewater are mixed with other wastewater (such as domestic sewage and other drainage), the maximum allowable discharge concentration of pollutants at the wastewater discharge outlet Calculated according to Appendix A. The maximum allowable displacement per ton of product must be measured at the discharge outlet of each workshop. 4.4.4 Sludge, solid waste and waste liquid should be disposed of reasonably. Table 1 Maximum allowable emission limits of water pollutants from caustic soda enterprises (enterprises constructed before January 1, 1989) Project
Production method
Level
First level
Mercury Electrolysis method
Separator electrolysis method
Ion exchange membrane electrolysis method
Production method
Carbide method
Ethylene oxide
Chlorination method| |tt||Wastewater category
Level 2
Level 3
Level 1
Level 2
Level 3
Level 1|| tt||Level 2
Level 3
Mercury
0.05
0.05
0.05
Maximum allowable discharge liquid concentration, mg/L
Asbestos
50
70
70
Activated chlorine||tt| |10
10
10
35
35
35
10
10
10
suspended solids
100
150
300
100
200
300
100| | tt | | 200 | ||Level
First level
Carbide wastewater
Polyethylene wastewater
Polycyanoethylene wastewater
Second level
Level three| |tt||Level 1
Level 2
Level 3
Level 1
Level 3
Level 3
Total Mercury Vinyl Chloride
0. 05
0.05
0.05
5
10
10bzxZ.net
Maximum allowable emission concentration, mg/ L
Chemical Oxygen Demand
(CODe.)
150
200
500
100
150| |tt||500
biochemical oxygen demand
(BOD,)
60
80
300
30||tt ||60
300
ton product displacement
m/t
2
2
pH value
6 ~9
tons of product
suspended solids
100
250
400
100
250||tt| |400
100
200
400
Sulfide
1
2
: com displacement||tt ||m*/t
7
pH value
6~9
production method
mercury electrolysis method
diaphragm electrolysis method
Project
Level
GB15581-95
Table 3 Maximum allowable discharge limits of water pollutants from caustic soda enterprises (January 1, 1989 to June 30, 1996 Enterprises built on a daily basis) maximum allowable emission concentration, mg/L
mercury
Level 1
Level 2
Level 3
Level 1||tt ||Level 3
Level 3
Level
Ion exchange membrane electrolysis method
Production method, wastewater category
Level 3
Level 3 Grade
0.005
0.005
0.005
Asbestos
60
50
70
Reactive Oxygen
5
5
5
35
35
35
5
5|| tt||5
suspended solids
70
150
300
70
150
300||tt ||70
150
300
Table 4
Maximum allowable emission limits of water pollutants from polyethylene enterprises (January 1, 1989 to June 1996 Enterprises constructed on the 30th) Project
Level
First Class
Carbide Wastewater
Carbide Method
Polyfluoroethylene Wastewater
Ethylene Oxygen
Chlorination method
Polyvinyl chloride wastewater
Level 3
Level 3
Level 1
Level 2
Level 3
Level 1
Level 2
Level 3
Total mercury
0.03
0.03
0.03|| tt||Vinyl chloride
2
5
2
2
5
Maximum allowable emission concentration, mg/L| |tt||Chemical Oxygen Demand
(CODer)
100
150
500
80
100||tt| |500
Biochemical oxygen content
(BOD,)
60
80
250
30
60
250
ton product displacement
m/t
1.5
7
1.5
PH value||tt ||6~9
tons of product
suspended solids
70
200
400
70
200| |tt||400
70
150
350
Sulfide
1
2|| tt||Discharge
m*/t
8
5
pH value
6~9
Production method||tt ||Diaphragm electrolysis
Project
Level
First level
Level 3
Level 3
Level 1
Ion exchange membrane electrolysis
Level 3
Level 3
GB15581--95
Table 5 Maximum allowable emission limits of water pollutants from caustic soda enterprises (July 1996 Enterprises constructed from the 1st) Maximum allowable emission concentration, mg/L
Asbestos
50
50
70
Measurable chlorine||tt ||20
20
20
2
2
2
suspended matter
70||tt| 150
300
70
100
300
Enterprises under construction since July 1st) Project
, Wastewater Category
Production Method
Carbide Wastewater
Carbide Method
Polyred Ethylene Wastewater|| tt | Level 1
Level 3
Level 3
Level 1
Level 3
Level 3
Level 1
Two Level
Level 3
Total mercury
0.005
0.005
0.005
Chlorine
2||tt ||2
2
2
2
2
Maximum allowable emission concentration, mg/L
Chemical oxygen demand| |tt||(CODcr)
100
150
500
80
100
500
Biochemical needs Oxygen
(BODs)
30
60
250
30
60
250||tt| |Tons of product drainage list
m\/t
5
1.5
pH value
6~9
tons of product
suspended solids
70
200
400|| tt||70
150
250
70
150
250
Sulfide
1||tt ||1
2
Drainage pH value
m*/t
6~9
Mercury, asbestos, active gas, chlorine should be Sampling should be done at the discharge outlet of the workshop wastewater treatment facility, and other pollutants should be sampled at the factory discharge outlet. All discharge outlets should be equipped with wastewater metering devices and discharge outlet signs. 5.2 Sampling frequency
The sampling frequency is determined according to the production cycle. If the production cycle is within 8 hours, sampling will be done every 2 hours. If the production cycle is greater than 8 hours, sampling will be done every 4 hours.
5.3 Production Statistics
The company's product output, raw material usage, etc. shall be based on the statutory monthly report or annual report. 5.4 Determination method
The determination method used in this standard is shown in Table 7.
Serial number
1
2
3
4
5
6
7|| tt||8
9
pH value
suspended solids
item
item
chemical oxygen demand CODcr||tt| |Sulfide
Mercury
Biochemical oxygen demand (BOD:)
Activated fluorine
Vinyl chloride
Asbestos
GB15581—95
Table 7 Determination methods
square
glass electrode method
gravimetric method
dichromate method
method||tt| |para-aminoditetraylaniline colorimetric method 1)
cold atomic absorption spectrophotometry
potassium permanganate-potassium persulfate digestion method
disulfide gland spectrophotometry| |tt||Dilution and inoculation method
N,N-diethyl-1,4-phenylenediamine titration method
N,N-diethyl-1,4-phenylenediamine Photometry
Gas Chromatography"
Gravimetry"
GB6920
GB11901
GB11914
GB7468
GB7469| | tt | | GB7488 | , after the relevant national method standards are promulgated, the national standards will be implemented temporarily. 2) The headspace gas chromatography method specified in Appendix B will be adopted temporarily. After the national method standards are published, the national standards will be implemented. 3) The gravimetric method will be implemented temporarily. After the national method standards are promulgated, the national standards will be implemented. Implement national standards. Standard implementation supervision
6
The environmental protection administrative departments of the people's governments at all levels are responsible for the supervision and implementation. In the formula: C-
GB15581-95||tt. ||Appendix A
Calculation method for the maximum allowable emission concentration of pollutants from the mixed wastewater discharge outlet (supplement)
=
2Q.C.+zQC
Q:+ Q
Q:=Wq
The maximum allowable emission concentration of pollutants, g/L, - the maximum allowable drainage volume of a certain product within a certain period of time, m\; Q
C||tt ||—the maximum allowable emission concentration of a certain pollutant for a certain product, mg/L; W,—a certain product—output within a certain period of time, t; q:-
-a certain product unit The maximum allowable drainage volume of production, m\/t; C, - the discharge concentration of a certain dye in other wastewater, g/L; Q, the drainage volume of other wastewater at a certain time, m. Note: 1=1,2. ,3,..** represents the type of wastewater in non-single product wastewater. j=1,2,3*, represents the i-th type of wastewater in other wastewater (domestic and non-production direct drainage). Appendix B
Determination method of vinyl chloride in water
Headspace gas chromatography
(supplement)
B1 instrument
B1.1 gas chromatograph , with FID detector. B1.2 constant temperature water bath, temperature control accuracy ±1°C. B1.3 gas-liquid balance tube (50mL colorimetric tube, total volume 75mL). B1.4 syringe: 1mL, 5mL syringe, 10~100ml. Micro syringe. B1.5
Medical anti-mouth rubber stopper.
B2 reagent
B2.1 methanol, superior grade pure.
B2.2 column carrier: GDX-103 (30~60 mesh). (A1)
(A2)
B2.3 vinyl fluoride, purity above 96%.
B2.4 Vinyl Chloride Standard Stock Solution: Take a 10mL volumetric flask and add about 9.8mL of methanol, leave it open for 10 minutes, and weigh to the nearest 0.1mg. Use a syringe with an air-tight valve to absorb 5 mL of vinyl chloride, and slowly inject it 5 mm above the methanol liquid level. Reweigh, dilute to volume, cover with stopper, shake spoon. Calculate the concentration of vinyl chloride based on the net weight increase, and then dilute it appropriately into an intermediate solution for later use. Step B3
Drawing of B3.1 standard curve
GB 15581--95
Take several 50mL colorimetric tubes, inject 75mL of pure water, and use a microsyringe to dispense different volumes of Put the intermediate solution in the colorimetric tube to make the concentrations 0.2.0.4, 0.6, 0.8, and 1.0g/L respectively. Seal with a reverse plug and tighten with thin wire. Pull out a long needle on the anti-mouth plug, with the needle tip at the 50mL mark, insert another short needle, and connect it to the ventilation system through a tee. Under constant pressure, introduce nitrogen into the colorimetric tube through the short needle, and water emerges from the long needle until the water level drops to the 50mL mark. Pull out the long needle immediately, stop ventilation, and pull out the short needle. Place the colorimetric tube into a -40°C constant temperature water bath to equilibrate for 40 minutes. Use a syringe preheated to 40°C to extract 1 mL of gas above the liquid, enter it into a chromatograph for analysis, and record the peak height. Each colorimetric tube can only be inhaled once. Also use pure water without adding sample to measure the blank and draw the concentration-peak height calibration curve. B3.2 Sampling
Flow the water sample smoothly into the 50mL colorimetric tube along the tube wall, fill it completely without leaving any space, plug the anti-mouth plug, tighten it with a thin wire, and bring it back to the experimental case.
B3.3 test
Drain the retrieved sample according to the above steps. After equilibrium at constant temperature, extract 1mL into the chromatograph for measurement and record the peak height. B3.4 Chromatographic conditions
Chromatographic column: $4mm×2m glass column, equipped with GDX-103. Column temperature: 50°C.
Detector temperature: 150℃.
Carrier gas: high purity nitrogen 50mL/min.
Hydrogen: 50mL/min.
Air: 500mL/min.
B3.5 calculation
vinyl chloride concentration (μg/L) blue C,
where: C, vinyl chloride standard solution concentration, g/Lh standard solution peak height, mm ;
h2—sample peak height with the same injection volume, mm. Additional notes:
This standard is proposed by the Science and Technology Standards Department of the National Environmental Protection Administration. h
h
This standard is drafted by the Standards Institute of the Chinese Academy of Environmental Sciences and the Jinxi Chemical Research Institute. The main drafters of this standard are Deng Fushan, Xia Qing, Cao Wanjun, and Qu Xiulan. The National Environmental Protection Administration is responsible for interpreting this standard. (B1)
)
Active fluorine
vinyl chloride
asbestos
GB15581—95
Table 7 Determination method
square
glass Electrode method
Gravimetric method
Dichromate method
method
para-aminoditetraylaniline colorimetric method 1)
cold atomic absorption spectrometry Photometry
Potassium permanganate-potassium persulfate digestion method
Disulfide gland spectrophotometry
Dilution and inoculation method
N,N-diethyl- 1,4-phenylenediamine titration
N,N-diethyl-1,4-phenylenediamine photometry
gas chromatography method"
gravimetric method"|| tt||GB6920
GB11901
GB11914
GB7468
GB7469
GB7488
Method source
GB11897||tt GB11898 For air chromatography, after the national method standard is published, the national standard will be implemented. 3) The gravimetric method will be adopted temporarily. After the national method standard is promulgated, the national standard will be implemented.
6
The environmental protection administrative departments of the people's governments at all levels are responsible for supervising the implementation. Formula: C-
GB15581-95
Appendix A
Calculation method for the maximum allowable discharge concentration of pollutants from mixed wastewater discharge outlets. (Supplement)
=
2Q.C.+zQC
Q:+Q
Q:=Wq
The maximum allowable emission concentration of pollutants , g/L, - the highest allowable discharge volume of a certain product within a certain period of time, m\; Q
C
- the highest allowable discharge concentration of a certain pollutant of a certain product, mg/L; W,—a certain product—output within a certain period of time, t; q:-
—the maximum allowable drainage volume per unit output of a certain product, m\/t; C,—a certain amount of other wastewater— The discharge concentration of dyes, g/L; Q, the drainage volume of other wastewater at a certain time, m. Note: 1=1,2,3, ..** indicates the type of wastewater in non-single product wastewater, j=1,. 2, 3*, indicating the i-th wastewater in other wastewater domestic and non-production direct drainage) Appendix B
Determination method of vinyl chloride in water
Headspace gas chromatography
( Supplement)
B1 instrument
B1.1 gas chromatograph with FID detector. B1.2 constant temperature water bath, temperature control accuracy ±1℃. B1.3 gas-liquid balance tube (50mL ratio. Color tube, total volume 75mL). B1.4 syringe: 1mL, 5mL syringe, 10~100ml. Micro syringe. B1.5
Medical anti-mouth rubber stopper.
B2 reagent
B2.1 methanol, superior grade pure.
B2.2 column carrier: GDX-103 (30~60 mesh). (A1)
(A2)
B2.3 vinyl fluoride, purity above 96%.
B2.4 Vinyl Chloride Standard Stock Solution: Take a 10mL volumetric flask and add about 9.8mL of methanol, leave it open for 10 minutes, and weigh to the nearest 0.1mg. Use a syringe with an air-tight valve to absorb 5 mL of vinyl chloride, and slowly inject it 5 mm above the methanol liquid level. Reweigh, dilute to volume, cover with stopper, shake spoon. Calculate the concentration of vinyl chloride based on the net weight increase, and then dilute it appropriately into an intermediate solution for later use. Step B3
Drawing of B3.1 standard curve
GB 15581--95
Take several 50mL colorimetric tubes, inject 75mL of pure water, and use a microsyringe to dispense different volumes of Put the intermediate solution in the colorimetric tube to make the concentrations 0.2.0.4, 0.6, 0.8, and 1.0g/L respectively. Seal with a reverse plug and tighten with thin wire. Pull out a long needle on the anti-mouth plug, with the needle tip at the 50mL mark, insert another short needle, and connect it to the ventilation system through a tee. Under constant pressure, introduce nitrogen into the colorimetric tube through the short needle, and water emerges from the long needle until the water level drops to the 50mL mark. Pull out the long needle immediately, stop ventilation, and pull out the short needle. Place the colorimetric tube into a -40°C constant temperature water bath to equilibrate for 40 minutes. Use a syringe preheated to 40°C to extract 1 mL of gas above the liquid, enter it into a chromatograph for analysis, and record the peak height. Each colorimetric tube can only be inhaled once. Also use pure water without adding sample to measure the blank and draw the concentration-peak height calibration curve. B3.2 Sampling
Smoothly flow the water sample into the 50mL colorimetric tube along the tube wall, fill it completely without leaving any space, plug the anti-mouth plug, tighten it with a thin wire, and bring it back to the experimental case.
B3.3 test
Drain the retrieved sample according to the above steps. After equilibrium at constant temperature, extract 1mL into the chromatograph for measurement, and record the peak height. B3.4 Chromatographic conditions
Chromatographic column: $4mm×2m glass column, equipped with GDX-103. Column temperature: 50°C.
Detector temperature: 150℃.
Carrier gas: high purity nitrogen 50mL/min.
Hydrogen: 50mL/min.
Air: 500mL/min.
B3.5 calculation
vinyl chloride concentration (μg/L) blue C,
where: C, vinyl chloride standard solution concentration, g/Lh standard solution peak height, mm ;
h2—sample peak height with the same injection volume, mm. Additional notes:
This standard is proposed by the Science and Technology Standards Department of the National Environmental Protection Administration. h
h
This standard is drafted by the Standards Institute of the Chinese Academy of Environmental Sciences and the Jinxi Chemical Research Institute. The main drafters of this standard are Deng Fushan, Xia Qing, Cao Wanjun, and Qu Xiulan. The National Environmental Protection Administration is responsible for interpreting this standard. (B1)
)
Active fluorine
vinyl chloride
asbestos
GB15581—95
Table 7 Determination method
square
glass Electrode method
Gravimetric method
Dichromate method
method
para-aminoditetraylaniline colorimetric method 1)
cold atomic absorption spectrometry Photometry
Potassium permanganate-potassium persulfate digestion method
Disulfide gland spectrophotometry
Dilution and inoculation method
N,N-diethyl- 1,4-phenylenediamine titration
N,N-diethyl-1,4-phenylenediamine photometry
gas chromatography method"
gravimetric method"|| tt||GB6920
GB11901
GB11914
GB7468
GB7469
GB7488
Method source
GB11897||tt GB11898 For air chromatography, after the national method standard is published, the national standard will be implemented. 3) The gravimetric method will be adopted temporarily. After the national method standard is promulgated, the national standard will be implemented.
6
The environmental protection administrative departments of the people's governments at all levels are responsible for supervising the implementation. Formula: C-
GB15581-95
Appendix A
Calculation method for the maximum allowable discharge concentration of pollutants from mixed wastewater discharge outlets. (Supplement)
=
2Q.C.+zQC
Q:+Q
Q:=Wq
The maximum allowable emission concentration of pollutants , g/L, - the highest allowable discharge volume of a certain product within a certain period of time, m\; Q
C
- the highest allowable discharge concentration of a certain pollutant of a certain product, mg/L; W,—a certain product—output within a certain period of time, t; q:-
—the maximum allowable drainage volume per unit output of a certain product, m\/t; C,—a certain amount of other wastewater— The discharge concentration of dyes, g/L; Q, the drainage volume of other wastewater at a certain time, m. Note: 1=1,2,3, ..** indicates the type of wastewater in non-single product wastewater, j=1,. 2, 3*, indicating the i-th wastewater in other wastewater domestic and non-production direct drainage) Appendix B
Determination method of vinyl chloride in water
Headspace gas chromatography
( Supplement)
B1 instrument
B1.1 gas chromatograph with FID detector. B1.2 constant temperature water bath, temperature control accuracy ±1°C. (50mL ratio. Color tube, total volume 75mL). B1.4 syringe: 1mL, 5mL syringe, 10~100ml. Micro syringe. B1.5
Medical anti-mouth rubber stopper.
B2 reagent
B2.1 methanol, superior grade pure.
B2.2 column carrier: GDX-103 (30~60 mesh). (A1)
(A2)
B2.3 vinyl fluoride, purity above 96%.
B2.4 Vinyl Chloride Standard Stock Solution: Take a 10mL volumetric flask and add about 9.8mL of methanol, leave it open for 10 minutes, and weigh to the nearest 0.1mg. Use a syringe with an air-tight valve to absorb 5 mL of vinyl chloride, and slowly inject it 5 mm above the methanol liquid level. Reweigh, dilute to volume, cover with stopper, shake spoon. Calculate the concentration of vinyl chloride based on the net weight increase, and then dilute it appropriately into an intermediate solution for later use. Step B3
Drawing of B3.1 standard curve
GB 15581--95
Take several 50mL colorimetric tubes, inject 75mL of pure water, and use a microsyringe to dispense different volumes of Put the intermediate solution in the colorimetric tube to make the concentrations 0.2.0.4, 0.6, 0.8, and 1.0g/L respectively. Seal with a reverse plug and tighten with thin wire. Pull out a long needle on the anti-mouth plug, with the needle tip at the 50mL mark, insert another short needle, and connect it to the ventilation system through a tee. Under constant pressure, introduce nitrogen into the colorimetric tube through the short needle, and water emerges from the long needle until the water level drops to the 50mL mark. Pull out the long needle immediately, stop ventilation, and pull out the short needle. Place the colorimetric tube into a -40°C constant temperature water bath to equilibrate for 40 minutes. Use a syringe preheated to 40°C to extract 1 mL of gas above the liquid, enter it into a chromatograph for analysis, and record the peak height. Each colorimetric tube can only be inhaled once. Also use pure water without adding sample to measure the blank and draw the concentration-peak height calibration curve. B3.2 Sampling
Smoothly flow the water sample into the 50mL colorimetric tube along the tube wall, fill it completely without leaving any space, plug the anti-mouth plug, tighten it with a thin wire, and bring it back to the experimental case.
B3.3 test
Drain the retrieved sample according to the above steps. After equilibrium at constant temperature, extract 1mL into the chromatograph for measurement, and record the peak height. B3.4 Chromatographic conditions
Chromatographic column: $4mm×2m glass column, equipped with GDX-103. Column temperature: 50°C.
Detector temperature: 150℃.
Carrier gas: high purity nitrogen 50mL/min.
Hydrogen: 50mL/min.
Air: 500mL/min.
B3.5 calculation
vinyl chloride concentration (μg/L) blue C,
where: C, vinyl chloride standard solution concentration, g/Lh standard solution peak height, mm ;
h2—sample peak height with the same injection volume, mm. Additional notes:
This standard is proposed by the Science and Technology Standards Department of the National Environmental Protection Administration. h
h
This standard is drafted by the Standards Institute of the Chinese Academy of Environmental Sciences and the Jinxi Chemical Research Institute. The main drafters of this standard are Deng Fushan, Xia Qing, Cao Wanjun, and Qu Xiulan. The National Environmental Protection Administration is responsible for interpreting this standard. (B1)
2 Constant temperature water bath, temperature control accuracy ±1°C. B1.3 gas-liquid balance tube (50mL colorimetric tube, total volume 75mL). B1.4 syringe: 1mL, 5mL syringe, 10~100ml. Micro syringe. B1.5
Medical anti-mouth rubber stopper.
B2 reagent
B2.1 methanol, superior grade pure.
B2.2 column carrier: GDX-103 (30~60 mesh). (A1)
(A2)
B2.3 vinyl fluoride, purity above 96%.
B2.4 Vinyl Chloride Standard Stock Solution: Take a 10mL volumetric flask and add about 9.8mL of methanol, leave it open for 10 minutes, and weigh to the nearest 0.1mg. Use a syringe with an air-tight valve to absorb 5 mL of vinyl chloride, and slowly inject it 5 mm above the methanol liquid level. Reweigh, dilute to volume, cover with stopper, shake spoon. Calculate the concentration of vinyl chloride based on the net weight increase, and then dilute it appropriately into an intermediate solution for later use. Step B3
Drawing of B3.1 standard curve
GB 15581--95
Take several 50mL colorimetric tubes, inject 75mL of pure water, and use a microsyringe to dispense different volumes of Put the intermediate solution in the colorimetric tube to make the concentrations 0.2.0.4, 0.6, 0.8, and 1.0g/L respectively. Seal with a reverse plug and tighten with thin wire. Pull out a long needle on the anti-mouth plug, with the needle tip at the 50mL mark, insert another short needle, and connect it to the ventilation system through a tee. Under constant pressure, introduce nitrogen into the colorimetric tube through the short needle, and water emerges from the long needle until the water level drops to the 50 mL mark. Pull out the long needle immediately, stop ventilation, and pull out the short needle. Place the colorimetric tube into a -40°C constant temperature water bath to equilibrate for 40 minutes. Use a syringe preheated to 40°C to extract 1 mL of gas above the liquid, enter it into a chromatograph for analysis, and record the peak height. Each colorimetric tube can only be inhaled once. Also use pure water without adding sample to measure the blank and draw the concentration-peak height calibration curve. B3.2 Sampling
Flow the water sample smoothly into the 50mL colorimetric tube along the tube wall, fill it completely without leaving any space, plug the anti-mouth plug, tighten it with a thin wire, and bring it back to the experimental case.
B3.3 test
Drain the retrieved sample according to the above steps. After equilibrium at constant temperature, extract 1mL into the chromatograph for measurement and record the peak height. B3.4 Chromatographic conditions
Chromatographic column: $4mm×2m glass column, equipped with GDX-103. Column temperature: 50°C.
Detector temperature: 150℃.
Carrier gas: high purity nitrogen 50mL/min.
Hydrogen: 50mL/min.
Air: 500mL/min.
B3.5 calculation
vinyl chloride concentration (μg/L) blue C,
where: C, vinyl chloride standard solution concentration, g/Lh standard solution peak height, mm ;
h2—sample peak height with the same injection volume, mm. Additional notes:
This standard is proposed by the Science and Technology Standards Department of the National Environmental Protection Administration. h
h
This standard is drafted by the Standards Institute of the Chinese Academy of Environmental Sciences and the Jinxi Chemical Research Institute. The main drafters of this standard are Deng Fushan, Xia Qing, Cao Wanjun, and Qu Xiulan. The National Environmental Protection Administration is responsible for interpreting this standard. (B1)
2 Constant temperature water bath, temperature control accuracy ±1°C. B1.3 gas-liquid balance tube (50mL colorimetric tube, total volume 75mL). B1.4 syringe: 1mL, 5mL syringe, 10~100ml. Micro syringe. B1.5
Medical anti-mouth rubber stopper.
B2 reagent
B2.1 methanol, superior grade pure.
B2.2 column carrier: GDX-103 (30~60 mesh). (A1)
(A2)
B2.3 vinyl fluoride, purity above 96%.
B2.4 Vinyl Chloride Standard Stock Solution: Take a 10mL volumetric flask and add about 9.8mL of methanol, leave it open for 10 minutes, and weigh to the nearest 0.1mg. Use a syringe with an air-tight valve to absorb 5 mL of vinyl chloride, and slowly inject it 5 mm above the methanol liquid level. Reweigh, dilute to volume, cover with stopper, shake spoon. Calculate the concentration of vinyl chloride based on the net weight increase, and then dilute it appropriately into an intermediate solution for later use. Step B3
Drawing of B3.1 standard curve
GB 15581--95
Take several 50mL colorimetric tubes, inject 75mL of pure water, and use a microsyringe to dispense different volumes of Put the intermediate solution in the colorimetric tube to make the concentrations 0.2.0.4, 0.6, 0.8, and 1.0g/L respectively. Seal with a reverse plug and tighten with thin wire. Pull out a long needle on the anti-mouth plug, with the needle tip at the 50mL mark, insert another short needle, and connect it to the ventilation system through a tee. Under constant pressure, introduce nitrogen into the colorimetric tube through the short needle, and water emerges from the long needle until the water level drops to the 50mL mark. Pull out the long needle immediately, stop ventilation, and pull out the short needle. Place the colorimetric tube into a -40°C constant temperature water bath to equilibrate for 40 minutes. Use a syringe preheated to 40°C to extract 1 mL of gas above the liquid, enter it into a chromatograph for analysis, and record the peak height. Each colorimetric tube can only be inhaled once. Also use pure water without adding sample to measure the blank and draw the concentration-peak height calibration curve. B3.2 Sampling
Flow the water sample smoothly along the tube wall into the 50mL colorimetric tube, fill it completely without leaving any space, plug the anti-mouth plug, tighten it with a thin wire, and bring it back to the experimental case.
B3.3 test
Drain the retrieved sample according to the above steps. After equilibrium at constant temperature, extract 1mL into the chromatograph for measurement, and record the peak height. B3.4 Chromatographic conditions
Chromatographic column: $4mm×2m glass column, equipped with GDX-103. Column temperature: 50°C.
Detector temperature: 150℃.
Carrier gas: high purity nitrogen 50mL/min.
Hydrogen: 50mL/min.
Air: 500mL/min.
B3.5 calculation
vinyl chloride concentration (μg/L) blue C,
where: C, vinyl chloride standard solution concentration, g/Lh standard solution peak height, mm ;
h2—sample peak height with the same injection volume, mm. Additional notes:
This standard is proposed by the Science and Technology Standards Department of the National Environmental Protection Administration. h
h
This standard is drafted by the Standards Institute of the Chinese Academy of Environmental Sciences and the Jinxi Chemical Research Institute. The main drafters of this standard are Deng Fushan, Xia Qing, Cao Wanjun, and Qu Xiulan. The National Environmental Protection Administration is responsible for interpreting this standard. (B1)
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