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[ Policies and Regulations of Chemical Machinery and Equipment Network ] In order to implement the "Environmental Protection Law of the People's Republic of China" and standardize the monitoring of the ecological environment, the Ministry of Ecology and Environment has organized the compilation of the National Ecological Environment Standard "Determination of Acrylic Acid in Water Quality by Ion Chromatography".
Opinions of relevant units
.
Feedback email zhiguanchu@mee.
gov.
cn, deadline before March 21, 2022
.
Chemical Machinery and Equipment Network Policies and Regulations Chemical Machinery and EquipmentOpinions of relevant units
.
Feedback email zhiguanchu@mee.
gov.
cn, deadline before March 21, 2022
.
In China's current ecological environment standards, the "Petrochemical Industry Pollutant Discharge Standard" (GB 31571-2015) and the "Synthetic Resin Industry Pollutant Discharge Standard" (GB 31572-2015) stipulate the discharge limit of acrylic acid in water , the emission limit of acrylic acid is 5mg/L, but there is no supporting monitoring and analysis method
.
.
In addition, Table A.
1 of Appendix A (Informative Appendix, Reference Index and Limit of Drinking Water Quality) of "Sanitation Standards for Drinking Water" (GB 5749-2006) stipulates that the limit of acrylic acid is 0.
5 mg/L, and no supporting facilities are provided.
monitoring and analysis methods
.
The "National Food Safety Standard for the Use of Additives for Food Contact Materials and Products" (GB 9685-2016) stipulates that the migration limit of acrylic acid and methacrylic acid is 6.
0 mg/kg, and no supporting monitoring and analysis methods are provided
.
"Workplace Hazardous Factors Occupational Exposure Limits Part 1: Chemical Hazardous Factors" (GBZ 2.
1-2019) stipulates that the time-weighted average allowable concentration (PC-TWA) limit of acrylic acid is 6 mg/m3, and its supporting analysis method is " Workplace Toxic Substances Determination of Carboxylic Acid Compounds" (GBZ/T 160.
59-2004), the detection method is solvent desorption-gas chromatography, and the detection limit is 100 mg/L
.
1 of Appendix A (Informative Appendix, Reference Index and Limit of Drinking Water Quality) of "Sanitation Standards for Drinking Water" (GB 5749-2006) stipulates that the limit of acrylic acid is 0.
5 mg/L, and no supporting facilities are provided.
monitoring and analysis methods
.
The "National Food Safety Standard for the Use of Additives for Food Contact Materials and Products" (GB 9685-2016) stipulates that the migration limit of acrylic acid and methacrylic acid is 6.
0 mg/kg, and no supporting monitoring and analysis methods are provided
.
"Workplace Hazardous Factors Occupational Exposure Limits Part 1: Chemical Hazardous Factors" (GBZ 2.
1-2019) stipulates that the time-weighted average allowable concentration (PC-TWA) limit of acrylic acid is 6 mg/m3, and its supporting analysis method is " Workplace Toxic Substances Determination of Carboxylic Acid Compounds" (GBZ/T 160.
59-2004), the detection method is solvent desorption-gas chromatography, and the detection limit is 100 mg/L
.
As an important basic raw material, acrylic acid is widely used, and its impact on the water body cannot be ignored.
However, since there is no corresponding national or industrial standard monitoring method in China, a standard method for the determination of acrylic acid in water quality is formulated to meet the requirements of petrochemical industry and synthetic resin industry.
The requirements of pollutant discharge standards are imperative
.
However, since there is no corresponding national or industrial standard monitoring method in China, a standard method for the determination of acrylic acid in water quality is formulated to meet the requirements of petrochemical industry and synthetic resin industry.
The requirements of pollutant discharge standards are imperative
.
This standard is formulated in order to implement the Environmental Protection Law of the People's Republic of China and the Water Pollution Prevention and Control Law of the People's Republic of China, prevent and control ecological environment pollution, improve the quality of the ecological environment, and standardize the determination method of acrylic acid in water
.
This standard specifies the ion chromatography method for the determination of acrylic acid in surface water, groundwater, domestic sewage and industrial wastewater
.
.
This standard specifies the ion chromatography method for the determination of acrylic acid in surface water, groundwater, domestic sewage and industrial wastewater
.
This standard is published for the first time
.
This standard is compiled with reference to HJ/T 91 Technical Specifications for Surface Water and Sewage Monitoring; HJ 91.
1 Technical Specifications for Sewage Monitoring; HJ 164 Technical Specifications for Groundwater Environmental Monitoring
.
.
This standard is compiled with reference to HJ/T 91 Technical Specifications for Surface Water and Sewage Monitoring; HJ 91.
1 Technical Specifications for Sewage Monitoring; HJ 164 Technical Specifications for Groundwater Environmental Monitoring
.
Method principle:
The acrylic acid in the sample enters the ion chromatography separation column with the eluent for separation, and is detected by a suppressed conductivity detector.
It is qualitatively determined according to the retention time, and the peak height or peak area is quantitatively determined
.
It is qualitatively determined according to the retention time, and the peak height or peak area is quantitatively determined
.
Instruments and Equipment:
1.
Sample bottle: brown polyethylene or other plastic material or glass material, with a volume of at least 40ml
.
2.
Ion chromatograph : with conductivity detector and suppressor
.
If gradient elution is used, it should be equipped with an online generation device for eluent or a gradient pump with more than two elements
.
3.
Chromatographic column
.
3.
1 Anion chromatographic column I: The filler is a polymer matrix such as polystyrene/divinylbenzene, with quaternary ammonium salt ion exchange group, equipped with corresponding anion protection column, or other equivalent anion chromatographic column, suitable for carbonate eluent
.
3.
2 Anion chromatography column II: The filler is polystyrene/divinylbenzene, polyethylvinylbenzene/divinylbenzene, with quaternary ammonium salt ion exchange group, equipped with corresponding anion protection column, or other equivalent anion chromatography Column, suitable for hydroxide eluent
.
4.
Syringe: 1ml～10ml
.
5.
Water-based needle-type microporous membrane filter : pore size 0.
45μm
.
6.
Suction filtration device: equipped with microporous membrane for use
.
7.
Ion purification column: Na type, Ag type and Ba type, specification 1g～2.
5g
.
8.
Hydrophobic organic purification column: C18 or similar purification column, specification 1g ~ 2.
5g
.
9.
General laboratory instruments and equipment
.
Chromatography filterSample bottle: brown polyethylene or other plastic material or glass material, with a volume of at least 40ml
.
2.
Ion chromatograph : with conductivity detector and suppressor
.
If gradient elution is used, it should be equipped with an online generation device for eluent or a gradient pump with more than two elements
.
3.
Chromatographic column
.
3.
1 Anion chromatographic column I: The filler is a polymer matrix such as polystyrene/divinylbenzene, with quaternary ammonium salt ion exchange group, equipped with corresponding anion protection column, or other equivalent anion chromatographic column, suitable for carbonate eluent
.
3.
2 Anion chromatography column II: The filler is polystyrene/divinylbenzene, polyethylvinylbenzene/divinylbenzene, with quaternary ammonium salt ion exchange group, equipped with corresponding anion protection column, or other equivalent anion chromatography Column, suitable for hydroxide eluent
.
4.
Syringe: 1ml～10ml
.
5.
Water-based needle-type microporous membrane filter : pore size 0.
45μm
.
6.
Suction filtration device: equipped with microporous membrane for use
.
7.
Ion purification column: Na type, Ag type and Ba type, specification 1g～2.
5g
.
8.
Hydrophobic organic purification column: C18 or similar purification column, specification 1g ~ 2.
5g
.
9.
General laboratory instruments and equipment
.
Collection of samples:
Collect samples in accordance with the relevant regulations of HJ/T 91, HJ 91.
1 and HJ 164
.
Collect at least 40 ml of sample in a sample vial (6.
1), fill the container with the sample and leave no head space
.
1 and HJ 164
.
Collect at least 40 ml of sample in a sample vial (6.
1), fill the container with the sample and leave no head space
.
Transport and storage of samples:
The collected samples should be refrigerated, transported and stored at 0 ℃ ~ 10 ℃, and measured within 2 days
.
If it is not possible to measure within this time, it can be frozen in a plastic bottle, and the measurement can be completed within 14 days
.
.
If it is not possible to measure within this time, it can be frozen in a plastic bottle, and the measurement can be completed within 14 days
.
Establishment of standard curve:
Accurately pipette 0.
00 ml, 0.
50 ml, 1.
00 ml, 5.
00 ml, 10.
00 ml, and 20.
00 ml of acrylic acid standard solution (5.
8) into six 50 ml volumetric flasks, dilute to the mark with water, and mix well
.
It is formulated into standard series of acrylic acid with mass concentrations of 0 mg/L, 0.
50 mg/L, 1.
00 mg/L, 5.
00 mg/L, 10.
0 mg/L and 20.
0 mg/L
.
The samples were injected in the order from low to high concentration, and the standard curve was established with the mass concentration of acrylic acid as the abscissa and the peak height (or peak area) as the ordinate
.
00 ml, 0.
50 ml, 1.
00 ml, 5.
00 ml, 10.
00 ml, and 20.
00 ml of acrylic acid standard solution (5.
8) into six 50 ml volumetric flasks, dilute to the mark with water, and mix well
.
It is formulated into standard series of acrylic acid with mass concentrations of 0 mg/L, 0.
50 mg/L, 1.
00 mg/L, 5.
00 mg/L, 10.
0 mg/L and 20.
0 mg/L
.
The samples were injected in the order from low to high concentration, and the standard curve was established with the mass concentration of acrylic acid as the abscissa and the peak height (or peak area) as the ordinate
.
Determination of sample:
The determination of the sample (7.
3) is carried out according to the same conditions and steps as the establishment of the standard curve (8.
2)
.
If the measurement result of the sample exceeds the range of the standard curve, it should be re-measured after dilution, and the dilution ratio D of the sample should be recorded at the same time
.
3) is carried out according to the same conditions and steps as the establishment of the standard curve (8.
2)
.
If the measurement result of the sample exceeds the range of the standard curve, it should be re-measured after dilution, and the dilution ratio D of the sample should be recorded at the same time
.
Precautions:
1.
When using the pretreatment purification column for purification treatment, if the resistance is large, a small volume syringe of 1 ml to 2 ml can be used to reduce the resistance and control the filtration flow rate
.
When using the pretreatment purification column for purification treatment, if the resistance is large, a small volume syringe of 1 ml to 2 ml can be used to reduce the resistance and control the filtration flow rate
.
2.
In order to avoid overloading the capacity of the chromatographic column, when analyzing samples of unknown concentration, it is best to dilute the injection first, and then select the appropriate dilution ratio or injection volume to protect the chromatographic column according to the obtained results
.
In order to avoid overloading the capacity of the chromatographic column, when analyzing samples of unknown concentration, it is best to dilute the injection first, and then select the appropriate dilution ratio or injection volume to protect the chromatographic column according to the obtained results
.
3.
If the chromatographic peak resolution decreases, the peak time of the analyte changes, or the peak shape changes, the reason may be that the column efficiency of the chromatographic column decreases, and it should be regenerated or replaced in time
.
If the chromatographic peak resolution decreases, the peak time of the analyte changes, or the peak shape changes, the reason may be that the column efficiency of the chromatographic column decreases, and it should be regenerated or replaced in time
.
This standard applies to the determination of acrylic acid in surface water, groundwater, domestic sewage and industrial wastewater
.
When the injection volume was 25μl, the detection limit of the method was 0.
08mg/L, and the lower limit of determination was 0.
32mg/L
.
.
When the injection volume was 25μl, the detection limit of the method was 0.
08mg/L, and the lower limit of determination was 0.
32mg/L
.
Original title: "Determination of Acrylic Acid in Water Quality by Ion Chromatography" Environmental Standards for Comments
