HJ 1058-2019Determination of ozone-depleting substances including CFC-12,HCFC-22,CFC-11 and HCFC-141b in rigid polyurethane foam and pre-blended polyether polyols -- Portable headspace/gas chromatography-mass spectrometry (English PDF)
硬质聚氨酯泡沫和组合聚醚中 CFC-12、HCFC-22 CFC-11 和 HCFC-141b 等消耗臭氧层物质的测定 便携式顶空气相色谱-质谱法
This is a limited preview
Buy now to download the full PDF (7 pages)
Need quotation for your management?
Get a formal quotation for HJ 1058-2019 in 30 minutes.
Issued by
Ministry of Ecology and Environment
Level / Type
National · Mandatory
Issue date
January 1, 1970
Implementation date
October 31, 2019
Scope
HJ 1058-2019 is the English-translated version of 硬质聚氨酯泡沫和组合聚醚中 CFC-12、HCFC-22 CFC-11 和 HCFC-141b 等消耗臭氧层物质的测定 便携式顶空气相色谱-质谱法.
HJ 1058-2019 — This standard specifies the determination of difluoromethylene chloride (CFC-12), difluoromethylene chloride in rigid polyurethane foam and combined polyethers.
Ozone depleting substances such as alkane (HCFC-22), monofluorotrichloromethane (CFC-11) and monofluorodichloroethane (HCFC-141b) Quality portable headspace/gas chromatography-mass spectrometry.
This standard applies to CFC-12, HCFC-22, CFC-11 and HCFC-141b in rigid polyurethane foams and combined polyethers. Qualitative detection.
When using rigid polyurethane foam as the test object, under the conditions specified in this standard, CFC-12, HCFC-22, CFC-11 the method detection limits for HCFC-141b and HCFC-141b are 2 µg, 2 µg, 2 µg, and 0.6 µg, respectively.
When the combined polyether is used as the test object, under the conditions specified in this standard, CFC-12, HCFC-22, CFC-11 and the method detection limits of HCFC-141b are 3 µg, 2 µg, 2 µg, and 0.9 µg, respectively.
Found what you need?
Document preview — HJ 1058-2019
National Standard of the People's Republic of China
- ICS
- 13.040.99
- Classification
- Z 15
Issued by: Ministry of Ecology and Environment
Contents
- Foreword
- 1 Scope
- 2 Methodology
- 3 Terms and definitions
- 4 Reagents and materials
- 5 Instruments and equipment
- 6 Sample
- 7 Analysis steps
- 8 Results representation
- 9 Quality Assurance and Quality Control
- 10 Waste disposal
- 11 Notes
- Appendix A (informative) Target ions and auxiliary ions of target compounds
- Appendix B (informative) Total ion chromatogram of target compound
Foreword
In order to implement the "Environmental Protection Law of the People's Republic of China" Environment, protect human health, regulate CFC-12, HCFC-22, CFC-11 and HCFC-141b and other ozone-depleting substances are determined by this standard.
This standard specifies CFC-12, HCFC-22, CFC-11 and HCFC-141b in rigid polyurethane foams and combined polyethers.
Determination of portable headspace/gas chromatography-mass spectrometry.
Appendix A and Appendix B of this standard are informative appendices.
This standard is issued for the first time.
This standard is formulated by the Department of Eco-Environmental Monitoring, Laws and Standards Department of the Ministry of Ecology and Environment.
This standard was drafted. China Environmental Monitoring Station.
Verification units of this standard. National Environmental Analysis and Testing Center, Zhejiang Environmental Monitoring Center, Shandong Province Ecological Environment Monitoring Center, Guangdong Environmental Monitoring Center, Tianjin Ecological Environment Monitoring Center and Chongqing Ecological Environment Monitoring Center.
This standard was approved by the Ministry of Ecology and Environment on October 31, 2019.
This standard will be implemented from October 31, 2019.
This standard is explained by the Ministry of Ecology and Environment.
CFC-12, HCFC-22, CFC-11 in rigid polyurethane foam and combination polyether and ozone depleting substances such as HCFC-141b and portable headspace/gas phase color Spectrum-mass spectrometry Warning. The standard used in this method is volatile and toxic chemicals. Protective equipment should be worn in accordance with requirements.
Avoid inhalation or contact with skin and clothing.
1 Scope
This standard specifies the determination of difluoromethylene chloride (CFC-12), difluoromethylene chloride in rigid polyurethane foam and combined polyethers.
Ozone depleting substances such as alkane (HCFC-22), monofluorotrichloromethane (CFC-11) and monofluorodichloroethane (HCFC-141b) Quality portable headspace/gas chromatography-mass spectrometry.
This standard applies to CFC-12, HCFC-22, CFC-11 and HCFC-141b in rigid polyurethane foams and combined polyethers.
Qualitative detection.
When using rigid polyurethane foam as the test object, under the conditions specified in this standard, CFC-12, HCFC-22, CFC-11 the method detection limits for HCFC-141b and HCFC-141b are 2 µg, 2 µg, 2 µg, and 0.6 µg, respectively.
When the combined polyether is used as the test object, under the conditions specified in this standard, CFC-12, HCFC-22, CFC-11 and the method detection limits of HCFC-141b are 3 µg, 2 µg, 2 µg, and 0.9 µg, respectively.
2 Method principle
Under a certain temperature condition, the target compound in the sample in the headspace bottle volatilizes to the liquid (solid) space, resulting in a certain the vapor pressure and gas-liquid (solid) two-phase dynamic equilibrium are reached. The target compound in the gas phase is purged with high purity carrier gas and adsorbed on in the built-in loop of a portable gas chromatography-mass spectrometer, the target compound in the loop is blown back into the carrier gas with high purity.
After separation by gas chromatography, it was detected by a mass spectrometer and qualitatively compared with the retention time and mass spectrum of a standard substance.
3 Terms and definitions
The following terms and definitions apply to this standard.
Rigid polyurethane foam Abbreviated as polyurethane rigid foam, it uses isocyanate and polyether as the main raw materials. It is widely used in foaming agents, catalysts, flame retardants, etc.
Under the action of additives, high-molecular polymers that are mixed by special equipment and foamed on-site by high-pressure spraying.
Pre-blended polyether polyols the mixture is composed of monomer polyether, foaming agent, cross-linking agent, catalyst, foam stabilizer and other components. Production hard One of the two-component raw materials of high quality polyurethane foam, commonly known as white material.
Ozone-depleting substances Chemicals that have a destructive effect on the ozone layer and are included in the China List of Controlled Ozone Depleting Substances.
4 Reagents and materials
Unless otherwise specified, analytical reagents that meet national standards are used. Experimental water is free of target compounds of distilled water or water prepared by pure water equipment.
4.1 Difluoromethylene chloride (CFC-12) standard solution. commercially available certified standard solution, the solvent is methanol.
4.2 Difluoromonochloromethane (HCFC-22) standard solution. commercially available certified standard solution, the solvent is methanol.
4.3 Monofluorotrichloromethane (CFC-11) standard solution. commercially available certified standard solution, the solvent is methanol.
4.4 Monofluorodichloroethane (HCFC-141b) standard solution. commercially available certified standard solution, the solvent is methanol.
4.5 Carrier gas. nitrogen, purity >=99.999%.
5 Instruments and equipment
5.1 Portable gas chromatograph-mass spectrometer. with loop injection function. The chromatographic part has the function of program temperature rise, the mass spectrometry part Electron Impact (EI) Ionization Source with 70 eV, with NIST Mass Library, Full Scan (SCAN), Manual/Auto Dynamic tuning, data acquisition and library search.
5.2 Headspace sampler. can be directly connected to the chromatographic section, and the sample can be purged to the portable gas chromatography-mass spectrometer by carrier gas Instrument inside the host.
5.3 Capillary column. 30 m × 0.32 mm, 1.0 m film thickness (100% polyethylene glycol), or 10 m × 0.1 mm, 0.2 m film thickness (100% polyethylene glycol). Other equivalent capillary columns can also be used.
5.4 Pipette. 20 µl, 5 ml or 10 ml.
5.5 Utility knife. metal.
5.6 Medicine spoon. metal material.
5.7 Sample vial. 40 ml brown screw-top glass bottle, Teflon-lined silicone rubber pad, or with headspace sampler (5.2) Matching glass bottles.
5.8 Sampling spoon. long handle, metal material.
5.9 General laboratory instruments and equipment.
6 Samples
6.1 Sample collection and storage
Rigid polyurethane foam. For each batch of foam products, 3 packaging units are randomly selected for sample collection; when packaging when there are less than 10 units, 1 or 2 packaging units can be selected for sample collection as appropriate. Collect 2 samples per packaging unit, One for analysis and one for preservation. When collecting samples, use a utility knife (5.5) on any of the rigid polyurethane foam Take a cube whose length, width and height are not less than 10 cm. If the sample cannot be tested on site, it should be at room temperature.
Transported and stored under light-proof and sealed condition, the test was completed within 10 days.
Note. If rigid polyurethane foam with a length, width and height of not less than 10 cm cannot be collected on site, the sample size can be adjusted according to the actual situation.
The product volume meets at least the requirements of 6.2 sample preparation.
Combination polyether. For each batch of combination polyether, randomly select 3 packaging units for sample collection; when there are few packaging units at 10 hours, 1 ~ 2 packaging units can be selected for sample collection as appropriate. Collect 2 samples per packaging unit, 1 for analysis, 1 for sample retention. When collecting samples, use a sampling spoon (5.8) to collect the combined polymer from the original storage container.
Ether, and then slowly introduce the sample from the sampling spoon into the sample bottle (5.7) along the wall until it is full and leaves no space. When sampling Minimize or reduce sample exposure to air. The samples should be analyzed as soon as possible after collection. If the samples cannot be tested on site, it should be transported and stored under normal temperature and protected from light. The test is completed within 10 days.
6.2 Preparation of test specimens
Rigid polyurethane foam sample. Use a utility knife (5.5) to cut a volume of about 1 cm3 (length, width, and height are 1 cm) Left and right) cubes and put them into the sample bottle (5.7) as soon as possible, all 6 sides of the cube must be new cutouts, to ensure 6 flat the surface was not in contact with the ambient air before cutting. Try to avoid or reduce sample exposure to air during sampling.
Combined polyether sample. Add 10 ml of experimental water to the sample bottle (5.7), and then use a medicine spoon (5.6) to hold about 10 mg Combine left and right (approximately mung bean size) polyether samples in a sample bottle (5.7), seal the sample bottle quickly, shake immediately after mixing During analysis, try to avoid or reduce sample exposure to air when taking samples.
After the sample is collected, the test will be performed on site as soon as possible.
Note. The sample is detected by mass spectrometry. If the target compound has a flat-headed peak, which affects the qualitative judgment of the adjacent target compound, the amount of sample should be reduced or re-measure the sample after dilution.
6.3 Blank sample
When testing rigid polyurethane foam samples. Replace the sample with ambient air as a blank sample.
When testing combined polyether samples. Use experimental water instead of samples as blank samples.
7 Analysis steps
7.1 Instrument reference conditions
7.1.1 Headspace injection reference conditions
Heating equilibration temperature. 50 °C; heating equilibration time. 10 min; sampling needle temperature. 60 °C; transmission line temperature. 60 °C; quantitative the ring volume is.200 µl or 400 µl.
7.1.2 Gas chromatography reference conditions
Program temperature increase. keep it at 50 °C for 3 minutes, increase it to 180 °C at 25 °C/min, and keep it for 3 minutes;
Set according to the instrument's instruction manual.
7.1.3 Mass spectrometry reference conditions
Scanning range. 41 ~ 300 amu; Ionization energy. 70 eV; Scanning method. Full scan (SCAN); Other parameters Set according to the instrument instruction manual.
See Figure B in Appendix B for the total ion chromatogram obtained by measuring the standard solution of the target compound under the reference conditions.
7.2 Calibration
7.2.1 Instrument performance check
After starting up, first check the instrument performance of the GC-MS system and run the corresponding check according to the instrument manual.
In order to ensure the accuracy of the test results, the mass spectrometry function should be tuned after starting up or running continuously for 12 hours.
Instrument use requirements.
7.2.2 Establishment of Qualitative Conditions for Target Compounds
Dilute the standard solution (4.1 ~ 4.4) with experimental water to prepare the target compound with a concentration of.200 µg/L.
standard solution. Analyze according to the instrument reference conditions (7.1) to obtain the retention time and standard quality of each target compound Spectrogram.
7.3 Sample determination
Measure the prepared sample (6.2) according to the instrument conditions (7.1).
Note. After analyzing a high-content sample, one or more blank samples should be analyzed for cross-contamination. If cross-contamination occurs, Bake the instrument pipeline and other corresponding measures to confirm that there is no contamination before continuing the test.
7.4 Blank test
The blank sample (6.3) is measured under the same instrument conditions as the sample measurement (7.3).
8 Result representation
8.1 Qualitative analysis
Compare the retention time (RT) of the target compound in the sample, the ratio of the auxiliary ion and the target ion abundance with the standard sample.
Qualitative. The target ion and auxiliary ion of the target compound are detailed in Appendix A.
The calibration solution should be analyzed on-site to obtain the retention time of the target compound.
The retention time deviation of the solution should not be greater than 10 s.
All ions with a relative abundance greater than 30% in the standard mass spectrum of the target compound should be present in the sample mass spectrum.
The relative abundance deviation of the above-mentioned characteristic ions in the mass spectrum and the standard mass spectrum should be within ± 30%. If the actual sample exists Show the background interference, the background effect should be deducted when comparing.
8.2 Results representation
Results are expressed as "checked out" or "not checked out."
9 Quality Assurance and Quality Control
9.1 Prior to the determination of each sample, a blank sample (6.3) shall be analyzed. The target compound shall not be detected in the blank sample.
9.2 Every 10 samples or each batch of samples (<=10 samples/batch) should be analyzed in a parallel sample.
Consistent.
10 Waste treatment
The waste liquid and waste generated in the experiment should be collected centrally, be marked accordingly, and be entrusted to a qualified unit for processing.
11 Matters needing attention
The sampling tools should be thoroughly washed before use. When collecting samples from different packaging units, pay attention to cleaning or replacing sampling workers.
With.
Appendix A
(Informative appendix) Target ion and auxiliary ion of target compound
Table A gives the Chinese and English names, target ions, and auxiliary ions of the target compound in the order of the peaks.
Table A Target ions and auxiliary ions of target compounds
Peak
order
Target compound
Chinese name
Target compound
English name
CAS number type
Target ion
Auxiliary ion
Difluoromethylene chloride (CFC-12) Difluorodichloromethane 75-71-8 Target compounds 85 87, 50, 101 Difluoromethane (HCFC 22) Difluorochloromethane 75-45-6 Target compounds 51 67, 69, 50 Monofluorotrichloromethane (CFC-11) Trichloromonofluoromethane 75-69-4 Target compounds 101 103, 105, 66 Monofluorodichloroethane (HCFC 141b) 1,1-Dichloro-1-fluoroethane 1717-00-6 Target compound 81 83, 61, 101 Appendix B (Informative appendix) Total ion chromatogram of target compound 1-difluoromethylene chloride (CFC-12); 2-difluoromonochloromethane (HCFC-22); 3-monofluorotrichloromethane (CFC-11);
4-monofluorodichloroethane (HCFC-141b)
Figure B Total ion chromatogram of a 50 µg target compound
......
This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 7 pages — is available in the English PDF.
Referenced standards
How to Download HJ 1058-2019
- 1
Add to cart
Click "Download PDF" on this page and choose "Buy this standard". You can add more standards before checkout.
- 2
Checkout
Enter your email and billing details. Payment is processed securely by Stripe (cards or bank transfer). Prefer bank details? Request a quotation (min. order $300).
- 3
Instant delivery (0–9 sec)
Delivery is automatic: within seconds of payment you'll receive an email with a secure download link. The link stays valid for 72 hours.
- 4
Invoice included
A tax invoice is attached to the confirmation email. Need a custom invoice? Contact us.
Related Standards
HJ 1409-2025 — Technical guidelines for environmental impact assessment - Marine ecology and environment
HJ 1410.1-2025 — Basic dataset of derivation of water quality criteria for aquatic organisms - Part 1: General principles
HJ 1410.10-2025 — Basic dataset of derivation of water quality criteria for aquatic organisms - Part 10: Mollusca
Secure payment via Stripe
Payments accepted
HJ 1058-2019
$165.00