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HJ 1057-2019 English PDF

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HJ 1057-2019: Determination of ozone-depleting substances including HCFC-22,CFC-11 and HCFC-141b in pre-blended polyether polyols -- Headspace/gas chromatography-mass spectrometry
Status: Valid

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HJ 1057-2019	English	329	Add to Cart	3 days [Need to translate]	Determination of ozone-depleting substances including HCFC-22,CFC-11 and HCFC-141b in pre-blended polyether polyols -- Headspace/gas chromatography-mass spectrometry	Valid	HJ 1057-2019

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Basic data

Standard ID	HJ 1057-2019 (HJ1057-2019)
Description (Translated English)	Determination of ozone-depleting substances including HCFC-22,CFC-11 and HCFC-141b in pre-blended polyether polyols -- Headspace/gas chromatography-mass spectrometry
Sector / Industry	Environmental Protection Industry Standard
Classification of Chinese Standard	Z15
Classification of International Standard	13.040.99
Word Count Estimation	14,112
Date of Issue	2019
Date of Implementation	2019-10-31
Issuing agency(ies)	Ministry of Ecology and Environment

HJ 1057-2019: Determination of ozone-depleting substances including HCFC-22,CFC-11 and HCFC-141b in pre-blended polyether polyols -- Headspace/gas chromatography-mass spectrometry

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(Determination of ozone depleting substances such as HCFC-22, CFC-11 and HCFC-141b in combined polyethers. Headspace/gas chromatography-mass spectrometry) National Environmental Protection Standard of the People's Republic of China HCFC-22, CFC-11 and HCFC-141b in polyethers Determination of ozone-depleting substances. Headspace/gas chromatography-mass spectrometry Determination of ozone-depleting substances including HCFC-22, CFC-11 and HCFC-141b in pre-blended polyether polyols-Headspace/gas chromatography-mass spectrometry 2019-10-31 released 2019-10-31 Implementation Released by the Ministry of Ecology and Environment

Foreword ... ii 1 Scope ... 1 2 Methodology ... 1 3 Terms and definitions ... 1 4 Reagents and materials ... 1 5 Instruments and equipment ... 2 6 Sample ... 2 7 Analysis steps ... 3 8 Calculation and Representation of Results ... 5 9 Precision and accuracy ... 6 10 Quality Assurance and Quality Control ... 7 11 Waste disposal ... 7 12 Notes ... 7 Appendix A (informative) Reference chromatograms ... 8 Appendix B (informative) Target component quantification and qualifier ion ... 9 Appendix C (informative) Method precision and accuracy ... 10

Foreword

In order to implement the "Environmental Protection Law of the People's Republic of China" Environment, protect human health, and regulate ozone depleting substances such as HCFC-22, CFC-11 and HCFC-141b in combined polyethers The determination method was formulated in this standard. This standard specifies the determination of HCFC-22, CFC-11, HCFC-141b and other ozone-depleting substances in combined polyethers. Air/gas chromatography-mass spectrometry. Appendix A, Appendix B and Appendix C 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 Province Environmental 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. Combined ozone depleting substances such as HCFC-22, CFC-11 and HCFC-141b in polyether Headspace/gas chromatography-mass spectrometry Warning. The standards used in this method are volatile and toxic chemicals. The solution preparation process should be performed in a fume hood; Wear protective equipment as required to avoid inhalation or contact with skin and clothing.

1 Scope

This standard specifies the determination of difluoromonochloromethane (HCFC-22), monofluorotrichloromethane (CFC-11) and Headspace/gas chromatography-mass spectrometry of ozone-depleting substances such as monofluorodichloroethane (HCFC-141b). This standard applies to the determination of ozone depleting substances such as HCFC-22, CFC-11 and HCFC-141b in combined polyethers. When the sample size is 1g, the detection limits of the methods for the determination of HCFC-22, CFC-11 and HCFC-141b are 0.2 µg/g, the lower limit of determination is 0.8 µg/g.

2 Method principle

At a certain temperature, the target components in the sample in the headspace bottle are volatilized to the headspace, generating a certain vapor pressure and Achieved gas-liquid two-phase dynamic equilibrium. The target components in the gas phase are separated by gas chromatography and detected by a mass spectrometer. Passed and Standards The material retention time was compared with the mass spectrum for qualitative analysis and quantification by internal standard method.

3 terms and definitions

The following terms and definitions apply to this standard. 3.1 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. 3.2 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 components Distilled water or water prepared by pure water equipment. 4.1 Methanol (CH3OH). chromatographically pure. 4.2 Monofluorotrichloromethane (CFC-11) standard solution. ρ (CFCl3) =.200 mg/L, the solvent is methanol, and the certificate is commercially available standard solution. 4.3 Standard solution of monofluorodichloroethane (HCFC-141b). ρ (CH3CFCl2) =.200 mg/L, the solvent is methanol. Certified standard solutions are sold. 4.4 Difluoromonochloromethane (HCFC-22) standard solution. ρ (CHF2Cl) =.200 mg/L, the solvent is methanol, and it is commercially available Certificate standard solution. 4.5 Internal standard standard solution. ρ (CH2BrCl) =.2000 mg/L, the solvent is methanol, and a commercially available certified standard solution. 4.6 4-Bromofluorobenzene (BFB). ρ = 25 mg/L, the solvent is methanol, and a commercially available certified standard solution. 4.7 Carrier gas. Helium, purity ≥99.999%.

5 Instruments and equipment

5.1 Gas chromatograph-mass spectrometer. The chromatographic part has a split/splitless inlet, which can be programmed to heat up; the mass spectrometer part has 70eV Electron bombardment (EI) ionization source with NIST mass spectrogram library with full scan (SCAN) and selective ion (SIM) scans Functions such as tracing, manual/auto tuning, data acquisition, quantitative analysis and library search. 5.2 Headspace sampler. The heating temperature control range is adjustable from room temperature to 120 ° C, and the temperature control accuracy is ± 1 ° C. 5.3 Chromatographic Column. Porous-layer open-tube capillary column, 60 m × 0.32 mm. Stationary phase is bonded silica or other equivalent capillary Tubing. 5.4 Analytical balance. Sensitivity 0.0001 g. 5.5 Sampling bottles. 40 ml brown screw-top glass bottles, polytetrafluoroethylene-lined silicone rubber pads, or other similar sampling bottles. 5.6 Headspace sample vials. glass headspace vials (20 ml), seals (PTFE/silicone), seal caps (screws) Screw caps or disposable caps), or glass headspace vials fitted with the headspace sampler (5.2). 5.7 Airtight syringe. 5 ml. 5.8 Glass cuvette. 10 ml. 5.9 Sampling spoon. long handle metal material. 5.10 Micro syringe. 2 μl ~ 500 μl. 5.11 Volumetric flask. Class A, 10 ml. 5.12 Instruments and equipment commonly used in general laboratories.

6 samples

6.1 Sample collection and storage For each batch of combination polyether, 3 packaging units are randomly selected for sample collection; when there are less than 10 packaging units, Samples can be taken from 1-2 packaging units as appropriate. Collect 2 samples per packaging unit, 1 for laboratory separation Analyze, and save 1 copy as a retained sample. When collecting samples, use a sampling spoon (5.9) to collect the combined polyether from the original storage container. Then, place the The sample is slowly introduced into the bottle along the wall of the sampling bottle (5.5) until it is full and leaves no space. Try to avoid or reduce samples when sampling The product is exposed to the air. The samples were transported and stored under normal temperature and protected from light, and the storage period did not exceed 10 d. 6.2 Preparation of test specimens Weigh approximately 1 g (accurate to 0.0001 g) of the sample into a glass cuvette (5.8), and make up to 10 ml with methanol (4.1) Mark the line and shake well. Use an airtight syringe (5.7) to draw 5.0 ml into the headspace sample vial (5.6) and add the internal standard After 100 µl of solution (4.5), wait for the test. 6.3 Preparation of blank samples Replace the sample with methanol (4.1) and prepare a blank sample following the same procedure as for sample preparation (6.2).

7 Analysis steps

7.1 Instrument reference conditions 7.1.1 Headspace injection reference conditions Sampling needle method. heating equilibrium temperature. 60C; heating equilibration time. 10 min; sampling needle temperature. 70C; injection Volume. 500 μl. Loop method. heating equilibrium temperature. 60C; heating equilibration time. 10 min; transmission line temperature. 100 ； C; fixed Measuring ring temperature. 110C; injection volume. 500 μl. 7.1.2 Gas chromatography reference conditions Inlet temperature. 240C; carrier gas. helium (4.7); injection mode. split injection (split ratio 10. 1); column flow (Constant current mode). 1.2 ml/min. Program temperature rise. keep 40C for 2.0 min, increase to 10C/min to 150C, and then 5C/min rises to.200C and keeps for 10.0 min. 7.1.3 Mass spectrometry reference conditions Ion source. electron bombardment (EI) source; ion source temperature. 230C; ionization energy. 70 eV; transmission line temperature. 250C; Quadrupole temperature. 150C. Scan method. Full scan (Scan). Scanning range. 45 amu ~ 180 amu. light Wire closing time. 19.0 min. See Figure A in Appendix A for the total ion chromatogram obtained from the standard solution of the target component under the reference conditions. 7.2 Calibration 7.2.1 Instrument performance check Using a micro-syringe (5.10), pipette 1.0 µl of 4-bromofluorobenzene solution (4.6) and feed it directly through the GC inlet. Sample, or add 20 µl of 4-bromofluorobenzene solution (4.6) to 5.0 ml of water and inject through the headspace sampler (5.2), After analysis by the mass spectrometer, the key ion abundance of the 4-bromofluorobenzene obtained should meet the requirements in Table 1. Otherwise, the parameters of the mass spectrometer need to be met. Adjust or clean the ion source. Table 1 4-Bromofluorobenzene key ion abundance standards Mass ion abundance standard 15% to 40% of mass 95 174 greater than 50% of mass 95 75 mass 30% to 60% of 95 175 mass 5% to 9% of 174 95 base peaks, 100% relative abundance 176 masses 95% to 101% of 174 mass 5% -9% of 96 mass 95 177 5% -9% of mass 176 173 less than 2% of mass 174-- 7.2.2 Drawing of calibration curve Use a micro-syringe (5.10) to transfer a certain amount of the target component standard solution (4.2 ~ 4.4) to a set of volumetric flasks (5.11). In medium, make up to the mark with methanol (4.1) and shake well. Use an air-tight syringe (5.7) to draw 5.0 ml each into the headspace In the sample bottle (5.6), then add 100 µl of the internal standard solution (4.5), and prepare the target component content of 5.00 µg, 10.0 µg, 20.0 µg, 50.0 µg, 100 µg, and.200 µg of internal standard content (reference concentration). According to the instrument reference conditions (7.1), measure from low content to high content in sequence, record the standard series of target components and the internal standard protection. Retention time, quantitation ion response value. 7.2.3 Calculation method of average relative response factor The relative response factor (RRFi) of a target component at point i in the standard series is calculated according to formula (1). IS IS RRF   (1) In the formula. RRFi--the relative response factor of a target component at point i in the standard series; Ai--Response value of a quantitative ion of a target component at the i-th point in the standard series; AISi--Response value of the quantifier ion of the internal standard in the standard series; ρIS--content of internal standard in standard series, μg; ρi--The content of a target component at the ith point in the standard series, μg. The average relative response factor RRF of a target component is calculated according to formula (2). RRF RRF  (2) Where. RRF--the average relative response factor of a target component; RRFi--the relative response factor of a target component at point i in the standard series; n-Standard series of points. 7.2.4 Calibration curve method The ratio of the content of the target component to the content of the internal standard is the abscissa, and the quantitative response of the target component is determined with the internal standard. The ratio of the measured ion response value is the ordinate, and a calibration curve is drawn. 7.3 Sample determination The sample (6.2) is measured in accordance with the instrument reference conditions (7.1). If the target component content in the sample is higher than the standard system The highest point content in the column shall be determined after the sample is appropriately diluted, and the dilution factor D shall be recorded at the same time. 7.4 Blank test Methanol (4.1) was used to replace the sample, and the blank sample was measured according to the same conditions and procedures as the sample measurement (7.3). set.

8 Results calculation and representation

8.1 Qualitative analysis Determine the target component based on the retention time and mass spectrum of the target component in the sample and the target component in the standard series. Sex. 8.1.1 Qualitative retention time Before sample analysis, establish a retention time window t ± 3S. t is the retention time of the target components at each concentration level during the initial calibration. Value, S is the standard deviation of the retention time of the target component at each concentration level during the initial calibration. When analyzing samples, the target components should be Peaks in the retention time window. 8.1.2 Characterization of Mass Ion Information All ions with a relative abundance greater than 30% in the standard mass spectrum of the target component should be present in the sample mass spectrum. The relative abundance deviation of the above-mentioned characteristic ions in the spectrum and the standard mass spectrum should be within ± 30%. If the actual sample is obvious Background interference. Background effects should be deducted when comparing. 8.2 Quantitative analysis After the target component is qualitatively identified, the average relative response factor or the calibration curve method is used for quantitative calculation. Target component See Table B in Appendix B for quantitative and qualifier ions. 8.2.1 Mean relative response factor method When calculated by the average relative response factor method, the mass concentration Cx of the target component in the sample is calculated according to formula (3). IS IS 2RRF x 1 ADV C = A m V       (3) In the formula. Cx-mass concentration of a target component in the sample, µg/g; Ax-response value of quantifier ion of a target component; AIS-response value of quantifier ion of internal standard; ρIS-content of internal standard, µg; RRF--the average relative response factor of a target component; D--The dilution factor of the sample. m--sample sampling volume, g; V1--constant volume in colorimetric tube, ml; V2--Liquid volume in headspace vial, ml. 8.2.2 Calibration curve method When using the calibration curve method, the mass concentration Cx of the target component in the sample is calculated according to formula (4). x 1 DV m V    (4) In the formula. Cx-mass concentration of a target component in the sample, µg/g; ρx-content of a target component obtained from the calibration curve, µg; D--sample dilution factor; m--sample sample size, g. V1--constant volume in colorimetric tube, ml; V2--Liquid volume in headspace vial, ml. 8.3 Representation of results The number of digits after the decimal point in the measurement result is the same as the detection limit of the method. A maximum of 3 significant digits are retained. According to requirements, the measurement results can also be reported in the form of mass percentage content.

9 Precision and accuracy

9.1 Precision Six laboratories performed 6 parallel determinations on 3 actual samples. Relative standard deviation in the laboratory is 0.7% ～ 19%; relative standard deviation between laboratories is 8.6% to 20%; repeatability limit is 2.5 µg/g to 2.17 × 104 µg/g; reproduction The property limit is 5.3 µg/g ～ 5.86 × 104 µg/g. For specific test results of method precision, see Table C.1 in Appendix C. 9.2 Accuracy Six laboratories performed spike recovery measurements on three actual samples with different target component contents. The average rate is 87.8% to 102%. For specific test results of the method accuracy, see Table C.2. In Appendix C. 10 Quality Assurance and Quality Control 10.1 Blank test At least one blank sample shall be analyzed for every 10 samples or batches (≤10 samples/batch). Target group in blank sample The fraction should not exceed the method detection limit. 10.2 Calibration The standard series requires at least 5 concentration levels (excluding zero concentration points). When using the average relative response factor method, The relative standard deviation (RSD) of the relative response factor (RRF) of the target component at each point of the standard series should be ≤20%; When quasi-curve method is used for calibration, the correlation coefficient of the curve should be ≥0.995. Otherwise, find the cause and redraw the calibration curve. In continuous analysis, the standard series of intermediate concentration points are analyzed every 24 hours, and the relative error between the measurement result and the standard value The difference is ± 20%. Otherwise, the calibration curve must be redrawn. 10.3 Parallel and matrix spiked samples Every 10 samples or batches (≤10/batch) should be analyzed for one parallel sample and matrix spike. Parallel knots The relative deviation of the fruit should be ≤30%, and the recovery rate of the matrix spike should be controlled between 60.0% ~ 120%. 10.4 Internal Standard The deviation between the retention time of the internal standard in the sample and the retention time of the internal standard in the calibration curve should not exceed 20s. The product change should be between 50% and.200%. 11 Waste treatment The waste liquid generated in the experiment should be collected in a centralized manner, be marked accordingly, and be entrusted to a qualified unit for processing. 12 Notes When collecting samples from different packaging units, pay attention to cleaning or replacing the sampling spoon.

Appendix A

(Informative appendix) Reference chromatogram Figure A shows the total ion chromatogram obtained by measuring the standard solution of the target component under the reference conditions. 6 8 10 12 14 16 18 20 Retention time (min) CH2BrCl (min) HCFC-22 CFC-11 HCFC-141b Figure A Total ion current chromatogram of a 50 µg target component standard solution

Appendix B

(Informative appendix) Target component quantification and qualifier Table B shows the quantitative and qualitative reference ions for the target components. Table B Target component quantifiers and qualifiers No. Target component type Quantitative ion Qualifier ion 1 HCFC-22 target components 51 67, 69, 50 2 CFC-11 Target components 101 103, 105, 66 3 HCFC-141b Target components 81 83, 61, 101 4 CH2BrCl Internal standard 130 128, 49, 93

Appendix C

(Informative appendix) Method precision and accuracy See Table C.1 and Table C.2. Table C.1 Method precision (actual samples) Target component Assay average / (µg/g) Relative in the laboratory standard deviation(%) Interlaboratory standard deviation(%) Repeatability limit r/(µg/g) Limit of reproducibility R/(µg/g) HCFC-22 200 2.2 ~ 12 13 34.9 77.6 17.3 1.2 ~ 15 20 3.5 10.3 370 1.2 ~ 15 14 62.9 157 CFC-11 196 1.5 ~ 5.0 8.6 19.0 50.3 17.3 1.6 ~ 8.9 10 2.5 5.3 1.15 × 103 1.5 ~ 10 19 191 629 HCFC-141b 578 0.7 ~ 19 17 175 322 82.3 2.0 ~ 4.4 8.9 7.0 21.5 2.08 × 105 0.9 ~ 6.1 9.5 2.17 × 104 5.86 × 104 Table C.2 Method accuracy (actual samples) Target component Original content / (µg/g) Standard content / (µg/g) Spike recovery P (%) Final spike recovery P ± 2 PS (%) HCFC-22 ND200 102 102 ± 23.6 ND17.3 87.8 87.8 ± 30.0 ND370 95.6 95.6 ± 23.4 CFC-11 ND196 100 100 ± 14.2 ND17.3 88.5 88.5 ± 11.4 1.15 × 103 1.55 × 103 91.9 91.9 ± 22.8 HCFC-141b 578 782 98.6 98.6 ± 31.6 82.3 58.5 91.8 91.8 ± 24.8 2.08 × 105 1.55 × 105 94.9 94.9 ± 26.2 Note. ND means not detected.

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