|
US$329.00 · In stock
Delivery: <= 3 days. True-PDF full-copy in English will be manually translated and delivered via email.
HJ 852-2017: Ambient air - Determination of indicative toxaphene - Gas chromatography mass spectrometry
Status: Valid
| Standard ID | Contents [version] | USD | STEP2 | [PDF] delivered in | Standard Title (Description) | Status | PDF |
| HJ 852-2017 | English | 329 |
Add to Cart
|
3 days [Need to translate]
|
Ambient air - Determination of indicative toxaphene - Gas chromatography mass spectrometry
| Valid |
HJ 852-2017
|
PDF similar to HJ 852-2017
Basic data | Standard ID | HJ 852-2017 (HJ852-2017) | | Description (Translated English) | Ambient air - Determination of indicative toxaphene - Gas chromatography mass spectrometry | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z15 | | Word Count Estimation | 14,117 | | Date of Issue | 2017-08-28 | | Date of Implementation | 2017-11-01 | | Regulation (derived from) | MEP Notice No. 41 | | Issuing agency(ies) | Ministry of Ecology and Environment | HJ 852-2017: Ambient air - Determination of indicative toxaphene - Gas chromatography mass spectrometry
---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
(Determination of Ambient Air Indicative Toxaphene by Gas Chromatography - Mass Spectrometry)
National Environmental Protection Standard of the People 's Republic of China
Determination of Ambient Air Indicative Toxaphene
Gas chromatography - mass spectrometry
Ambient air - Determination of spec toxaphene -
Gas chromatography mass spectrometry
2017-08-28 released
2017-11-01 implementation
Issued by the Ministry of Environmental Protection
i directory
Preface ..ii
1 Scope of application
2 normative reference documents
3 Principle of the method
4 reagents and materials 1
5 instruments and equipment 2
6 Sample 3
7 Analysis steps
8 Calculation and representation of results
9 precision and accuracy
Quality assurance and quality control
11 Waste treatment
Appendix A (informative) The names of three indicative fumaric, quantitative ions and auxiliary qualitative ions .10
Appendix B (informative) method of precision and accuracy 11
Foreword
In order to implement the Environmental Protection Law of the People's Republic of China and the Law of the People's Republic of China on the Prevention and Control of Atmospheric Pollution,
Protection of human health, regulate the ambient air poisoning fenfen determination method, the development of this standard.
This standard specifies the gas chromatography-mass spectrometry for the determination of three indicative toxaphene in ambient air.
This standard is the first release.
Appendix A and Appendix B of this standard are informative.
This standard is organized by the Environmental Monitoring Department of the Ministry of Environmental Protection and the Department of Science and Technology Standards.
The main drafting unit of this standard. Qingdao Environmental Monitoring Center Station.
The standard verification unit. the National Environmental Analysis and Testing Center, the Ministry of Agriculture Agricultural Product Quality Supervision, Inspection and Testing Center (Green
Island), Shandong Entry-Exit Inspection and Quarantine Bureau Inspection and Quarantine Technology Center, Chinese Academy of Sciences Qingdao Bio-Energy and Process Research Institute, Qingdao sea
Ocean Geology Institute and Qingdao University of Technology.
The environmental protection department of this standard approved on August 28,.2017.
This standard has been implemented since November 1,.2017.
This standard is explained by the Ministry of Environmental Protection.
Determination of Ambient Air Indicative Toxaphene by Gas Chromatography - Mass Spectrometry
WARNING. The organic solvents and standard solutions used in the experiments are toxic substances. The preparation of the solution and the preparation of the sample should
Fume hood, the operation should be required to wear protective equipment, to avoid contact with skin and clothing.
1 Scope of application
This standard specifies the gas chromatography-mass spectrometry for the determination of three indicative toxaphene in ambient air.
This standard is applicable to the determination of three indicative toxaphenes (P26, P50, P62) in ambient air.
When the extraction capacity of 500 m3 (standard state), the three kinds of indicative toxaphene P26, P50, P62 method detection limit
Do not 4 pg/m3, 4 pg/m3, 8 pg/m3, the lower limit of determination is 16 pg/m3, 16 pg/m3, 32 pg/m3.
2 normative reference documents
The contents of this standard refer to the following documents or their terms. Those who do not specify the date of the reference file, the effective version of the appropriate
For this standard.
Technical requirements and testing methods for HJ 93 ambient air particulate matter (PM10 and PM2.5) samplers
Technical Guidelines for Sampling of Semi - Volatile Organic Compounds for Environmental Air
3 Principle of the method
The poisonous fenfen in ambient air was collected on a quartz fiber filter and a polyurethane foam (PUF) with a large flow sampler,
With the appropriate organic solvent extraction, the extract was concentrated, the multi-layer acidic silica gel column and activated silica gel column purification, with gas chromatography
Separation of negative chemical source mass spectrometry for detection. The retention time and the characteristic ion abundance ratio were qualitative and the internal standard method was quantified.
4 reagents and materials
4.1 concentrated sulfuric acid. ρ (H2SO4) = 1.84 g/ml, excellent grade pure.
4.2 anhydrous sodium sulfate (Na2SO4). analytical grade.
Before use in the muffle furnace at 450 ℃ for 2 h, after cooling, stored in the grinding glass bottle in the dryer sealed.
4.3 Acetone (C3H6O). pesticide residues.
4.4 ether (C2H6O). pesticide residues.
4.5 n-Hexane (C6H14). Pesticide level.
4.6 Toluene (C7H8). Pesticide level.
4.7 Extract. A mixed solution of ether (4.4) and n-hexane (4.5), 5 95.
4.8 Eluent. A mixed solution of n-hexane (4.5) and toluene (4.6), 6535.
4.9 toxaphene standard solution. ρ = 5.0 μg/ml, the solvent is isooctane.
Containing the standard solution of poisonous fenfen P26, P50, P62, the direct purchase of certified standard solution.
4.10 Substitutes Standard solution. ρ = 1.0 μg/ml, solvent is nonane.
With 13C10-γ-chlordane as a substitute, the direct purchase of certified standard solution.
4.11 standard standard stock solution. ρ = 100 μg/ml, the solvent is methanol/toluene, 97 3.
With octachlorobenzene (OCN) as the internal standard, direct purchase of certified standard solution.
4.12 standard internal standard solution. ρ = 10.0 μg/ml.
2 Standardize the internal standard stock solution (4.11) with n-hexane (4.5) to 10.0 μg/ml.
4.13 Silica gel. for chromatography, 178-150 μm (80-100 mesh).
4.14 Activated silica gel. Silicone gel (4.13) was activated at 180 ° C for 6 h, cooled in a desiccator, stored in a clean grinding
The glass bottle is sealed and stored.
4.15 22% Acid Silica Gel. Activated Silica Gel (4.14) 78 g Sulfuric acid (4.1) 22 g was added dropwise,
Stored in a clean grinding glass bottle sealed.
4.16 44% Acid Silica Gel. Activated Silica Gel (4.14) 56 g After adding concentrated sulfuric acid (4.1) 44 g,
Stored in a clean wide-mouth glass bottle sealed to save.
4.17 quartz fiber filter. before use in the muffle furnace at 450 ℃ for 4 h, after cooling with aluminum foil wrapped, stored in the filter box,
Ensure that the filter is not contaminated before and after sampling and is in flattened before sampling.
The retention efficiency of 0.3 μm standard particles was not less than 99%, and when the air velocity was 0.45 m/s,
Force is not greater than 3.5 kPa, in this air velocity, the extraction of high efficiency filter purification of air 5 h, per square centimeter filter loss
Weighs no more than 0.012 mg.
4.18 Polyurethane foam (PUF). Polyether type, density 0.022 g/cm3, cut into cylindrical (diameter according to the sampling head
Glass sampling tube specifications to determine).
Before use, boil the hot water with hot, and then placed in warm water repeatedly scrub, dry with acetone (4.3) Soxhlet extraction 16 h,
And then extracted with ether/n-hexane (4.7) Soxhlet for 16 h, wrapped in aluminum foil washed with n-hexane (4.5), stored in
Dryer is saved. You can also purchase commercially available purified PUF.
4.19 Carrier gas. helium, purity 99.999%.
4.20 Reaction gas. methane gas, purity 99.999%.
Note 1. All of the above standard solutions are kept at or below 4 ° C or stored in the manufacturer's product description preservation method. Should be restored before use
To room temperature, mix well.
Note 2. Mixing in 4.15 and 4.16 is sufficient for rotary evaporators.
5 instruments and equipment
5.1 sampling device. the collection of air poisoning of the sampling device by the sampling head, sampler composition. The structure of each part of the sampling device
And performance requirements should meet the requirements of HJ 691.
5.1.1 Sampler. Sampler should have an automatic cumulative sampling volume, according to the temperature, air pressure automatically converted the cumulative standard sample sample
Product function; should have automatic timing, power and then restart the automatic compensation due to voltage fluctuations and resistance changes caused by changes in traffic
Function. In the case of filters and adsorbents, the load flow of the sampler should be capable of reaching 250 L/min or more
The flow rate is 225 L/min.
5.1.2 Sampling head. Sampling head by the sampling cutter, filter and filter support part, filled with adsorbent sampling tube, sampling cylinder
And silicone rubber seals, see Figure 1. Sampling head of the material should be used stainless steel or polytetrafluoroethylene and other non-adsorbed organic material
material. The sampling tube was made of borosilicate glass with an inner diameter of 60 mm and a length of 125 mm. The support of the adsorbent was a pore size of 1.2 mm
(16 mesh) stainless steel mesh. The performance parameters of the cutter and cutter shall be selected according to the requirements of the monitoring and the relevant standards.
The standard should meet the requirements of HJ 93.
5.1.3 Standard Flowmeter or Standard Accumulated Flowmeter. Standard Flowmeter or Standard Accumulated Flowmeter for Calibration Sampler
At least 180 to 260 L/min, the error within ± 2%.
3 Figure 1 Schematic diagram of the sampling head
5.2 Gas Chromatography/Mass Spectrometer. Chromatographic section with split/splitless inlet, electronic flow control and programmed temperature function;
Spectrum is a quadrupole mass spectrometer with a negative chemical source (NCI) with selective ion scanning mode (SIM), manual/auto tuning and
Library search and other functions.
5.3 Capillary column. column length 30 m, inner diameter 0.25 mm, film thickness 0.25 μm, stationary phase 5% phenyl 95% methyl polysiloxane stone
English capillary column, or other equivalent column.
5.4 column. the diameter of 20 mm, 350 mm long, with PTFE piston at the bottom of the glass column.
5.5 multi-layer acidic silica gel column. dry column, from bottom to top followed by glass wool, 44% acid silica gel (4.16) 12.5 g, 22%
Acid silica gel (4.15) 10.0 g, anhydrous sodium sulfate (4.2) 2 g. You can also buy a product column.
5.6 activated silica gel column. dry column, from bottom to top followed by glass wool, activated silica gel (4.14) 10.0 g, anhydrous sodium sulfate
(4.2) 2 g. You can also buy a product column.
5.7 Soxhlet extractor. 1000 ml, Soxhlet extractor should be matched with PUF diameter. Other properties may also be used
Extraction device.
5.8 Concentration device.
5.9 General laboratory instruments commonly used.
6 samples
6.1 Collection and storage of samples
The installation, calibration and sample collection and transportation of the sampler are carried out in accordance with the requirements of HJ 691. The sampling flow is generally set to
220 ~ 230 L/min. Add 50.0 μl of the substitute (4.10) to the PUF adsorbent prior to sampling.
4 samples after the collection of PUF and filter with aluminum foil were wrapped and then placed in the sample storage box, dark seal, and sent as soon as possible
Laboratory analysis. The samples were stored below 4 ° C and should be extracted within 7 days. The extract was analyzed within 40 days.
6.2 Preparation of Specimen
6.2.1 Extraction of samples
Place the sampled PUF together with the membrane in a 1000 ml Soxhlet extractor (5.7) and add 500 ml
The extract (4.7) was extracted at a rate of 4 to 5 cycles per hour for 18 h. After extraction, the extract was concentrated to 1 ml,
To be purified.
Note. Other methods of extraction and extraction of solvents may be used by experimentally demonstrating that the method requirements are met.
6.2.2 purification of the sample
6.2.2.1 multi-layer acidic silica gel column purification
First, 50 ml of n-hexane (4.5) was used to elute the multilayer acid silica gel column (5.5). When n-hexane was just close to the sodium sulfate layer,
The PTFE piston was closed and the concentrated extract (6.2.1) was then transferred to a multilayer acid silica gel column and 90 ml
N-hexane (4.5) elution rate of about 2.5 ml/min (about 1 drop/s), the eluate was collected and concentrated to 2 ml
The next step is to purify.
6.2.2.2 Activated silica gel column purification
The activated silica gel column (5.6) was eluted with 50 ml of n-hexane (4.5) until the n-hexane was close to the sodium sulfate layer
PTFE pistons, and the concentrated solution (6.2.2.1) eluted with the multilayer acid silica gel column was transferred to an activated silica column with 35 ml
Hexane (4.5) was rinsed and the eluent was discarded and eluted with 50 ml of eluent (4.8) at a rate of about 2.5 ml/min
About 1 drop/s), the eluate was collected, and the eluate was concentrated to 1 ml or less and then to 1.0 ml with n-hexane (4.5)
Finally add 5.0 μl of internal standard to use the solution (4.12), to be tested.
6.3 Preparation of full program blank samples
The sealed PUF and quartz fiber membranes were brought to the site and 50.0 μl of substitutes was added to the PUF adsorbent
(4.10), the sample is exposed to the scene but not sampling, after sampling with the same sample with aluminum foil were wrapped and then placed in the sample
Box, with the sample back to the laboratory, according to the same steps with the sample processing, made of the whole program blank sample,
And then with n-hexane (4.5) to 1.0 ml, and finally add 5.0 μl of the standard internal standard solution (4.12), to be tested.
7 Analysis steps
7.1 Instrument reference conditions
7.1.1 Gas Chromatographic Reference Conditions
Inlet temperature. 250 ° C; injection method. no split injection; injection volume. 1.0 μl; carrier gas flow rate. 1.0 ml/min;
Procedure temperature. 100 ° C (1 min) and water pressure at 15 ° C (2 min).
7.1.2 Mass spectrometry reference conditions
Negative chemical source (NCI). ion source temperature. 150 ° C; scanning range. m/z 50 ~ 450 amu; scanning mode. selection
Ion scanning (SIM). Transmission line temperature. 250 ° C; solvent delay time. 6.0 min. The rest of the parameters refer to the instrument use
Set the book. The reaction gas was methane gas and the flow rate was 1.5 ml/min.
7.2 Quantitative ions and auxiliary qualitative ions
Using the Selective Ion Mode (SIM) assay, the choice of quantitative and auxiliary qualitative ions for the target compound should be based on three
The indicated full-scan negative chemical source mass spectra of the indicative fenbuterol standard are also determined by reference to Table A.2 in Appendix A.
57.3 Calibration
7.3.1 Instrument tuning
After selecting the negative chemical source mode and the methane gas, the instrument adjusts the negative chemical source through the instrument software,
Establish calibration curves and make measurements.
7.3.2 Calibration curve
(4.9) and the substitute standard (4.10) were used to mix the standard dosage of toxaphene,
The concentration of (4.5) was 20.0 μg/L, 40.0 μg/L, 80.0 μg/L, 120 μg/L and.200 μg/L, respectively.
And the standard solution (4.12) was added to each concentration point in the calibration curve to make the concentration of the internal standard compound 50.0 μg/L,
According to the reference conditions of the instrument from low to high concentration in turn measured. Record the target compounds in the standard series, substitutes
And the retention time of the internal standard, the response value of the quantitative ion.
7.3.3 Calculation of average relative response factors
The relative response factor (iRRF) of the target compound in the standard series i is calculated according to equation (1)
is
is
RRF
(1)
Where. iRRF - the relative response of the target compound at point i in the standard series;
iA - the response value of the quantitation ions of the target compound at point i in the standard series;
siA - internal standard quantitative ion response value;
si__ - mass concentration of internal standard substance, g/L;
i - Mass concentration of the target compound in the standard series, g/L.
The average relative response factor (RRF) of the target compound is calculated according to equation (2)
RRF
RRF
1 (2)
Where. RRF - the average relative response of the target compound;
iRRF - the relative response of the target compound in the standard series;
n - standard series points.
RRF standard deviation (SD) calculated according to formula (3).
)( 2
RRFRRF
SD
(3)
The relative standard deviation (RSD) of RRF is calculated according to equation (4).
0 distance
RRF
SD
RSD (4)
7.3.4 Establish the calibration curve with the least squares method
is
isi
A
As the ordinate, the concentration (i) of the standard solution is abscissa, and the calibration is established by the least squares method
curve.
7.4 Determination
The test specimen (6.2.2.2) was measured under the same conditions as the calibration curve.
7.5 blank test
The whole program blank sample to be measured (6.3) was measured under the same conditions as the samples.
8 results are calculated and expressed
8.1 Standard reference chromatogram
Under the instrumentation conditions given in this standard (7.1), the indicative fenfenfen P26, P50, P62, internal standard and substitutes
The total ion chromatogram is shown in Fig.
Retention time (t)/min
1-13C10-γ-chlordane; 2-P26; 3-P50; 4-P62;
Figure 2 Total ion chromatogram of three indicative toxaphene, internal standard and substitutes
8.2 Qualitative analysis
7 According to the relative retention time of the target in the sample, the fragment ion mass ratio and the different ion abundance ratio were qualitative. In the sample
The relative retention time (RRT) of the labeled compound is between ± 0.06 and the relative retention time of the latest calibration standard. Targeting
The auxiliary qualitative ions of the compound should be present in the sample. The target qualitator and quantified ion peak area of the target compound in the sample
(Q-sample) relative to the calibration curve of the target compound and the quantified ion peak area (Q standard) relative deviation
Control within ± 30%.
The relative retention time (RRT) is calculated according to equation (5).
is
RT
RT
RRT (5)
Where. iRT - retention time of the target compound, min;
siRT - retention time of internal standard, min.
The ratio (Q) of the auxiliary qualitative ion to the quantified ion peak area of the target compound is calculated according to equation (6)
A Q (6)
Where. tA - auxiliary qualitative ion peak area;
qA - Quantitative ion peak area.
8.3 Quantitative analysis
8.3.1 Calculate the mass concentration (i) of the target compound in the sample by the average relative response factor according to equation (7).
isi
iis
ARRF
Aρ
ρ
(7)
Where. i - mass concentration of the target compound in the sample, μg/L;
iA - the response value of the target compound to quantify ions;
isA - the response value of the quantitation ion of the internal standard compound;
isbook - the mass concentration of the internal standard compound in the sample, μg/L;
iRRF - the average relative response of the target compound.
8.3.2 Mass concentration of the target compound in the sample () Calculated according to equation (8).
nd
fti
10DVρ
(8)
Where. - concentration of the target compound in ambient air, pg/m3;
i_2 - the mass concentration of the target compound in the sample from the average relative response factor or calibration curve, μg/L;
tV - volume of the sample after purification and concentration, ml;
8ndV - the sampling volume under standard conditions, m
3;
fD - dilution factor.
8.4 results show
Determination of the results should be reported P26, P50, P62 three kinds of indicative of the concentration of fenfen. When the result is less than 100
pg/m3, to the integer bit; when the determination is greater than or equal to 100 pg/m3, retain 3 significant digits.
9 precision and accuracy
9.1 precision
Six laboratories were added with three indicative toxaphene and substitutes at concentrations of 20.0 pg/m3, 100 pg/m3,.200 pg/m3
Of the samples were subjected to six replicates.
The relative standard deviations in the laboratory were 2.4% ~ 17%, 2.8% ~ 21%, 2.7% ~ 23%, respectively.
The relative standard deviations were 9.0% ~ 25%, 11% ~ 16% and 8.9% ~ 17%, respectively.
Repetitive limit r is. 4 ~ 6 pg/m3, 25 ~ 31 pg/m3, 36 ~ 68 pg/m3;
The reproducibility R is. 8 to 16 pg/m3, 41 to 49 pg/m3, and 56 to 104 pg/m3.
9.2 Accuracy
Six laboratories were added with three indicative toxaphene and substitutes at concentrations of 20.0 pg/m3, 100 pg/m3,.200 pg/m3
Of the samples were measured by spiked assays.
The recoveries were 71.3% ~ 132%, 67.5% ~ 115% and 70.1% ~ 113%, respectively.
The final recoveries were 99.9% ± 36.4% ~ 111% ± 56.0%, 88.0% ± 24.2% ~ 89.5% ± 28.8%
88.6% ± 16.2% ~ 92.3% ± 16.5%.
Details of precision and accuracy are given in Table B.1 and Table B.2 in Appendix B.
10 quality assurance and quality control
10.1 Calibration curve
The calibration curve requires at least 5 concentration points, the relative standard deviation of the standard series of target compound relative response factors (RRF)
(RSD) should be ≤ 20% or the calibration curve correlation coefficient ≥ 0.995.
10.2 full program blank
Each batch of samples should be made a blank test of the whole procedure, the measured value of the target compound in the blank should be lower than the method detection limit.
10.3 Calibration curve verification
For each 20 samples, a standard solution of the midpoint of the calibration curve was measured, and the measured value was the same as the calibration curve
Relative deviation should be ≤ 20%. Otherwise, a new calibration curve should be established.
10.4 Internal standard response and...
Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of HJ 852-2017_English be delivered?Answer: Upon your order, we will start to translate HJ 852-2017_English as soon as possible, and keep you informed of the progress. The lead time is typically 1 ~ 3 working days. The lengthier the document the longer the lead time. Question 2: Can I share the purchased PDF of HJ 852-2017_English with my colleagues?Answer: Yes. The purchased PDF of HJ 852-2017_English will be deemed to be sold to your employer/organization who actually pays for it, including your colleagues and your employer's intranet. Question 3: Does the price include tax/VAT?Answer: Yes. Our tax invoice, downloaded/delivered in 9 seconds, includes all tax/VAT and complies with 100+ countries' tax regulations (tax exempted in 100+ countries) -- See Avoidance of Double Taxation Agreements (DTAs): List of DTAs signed between Singapore and 100+ countriesQuestion 4: Do you accept my currency other than USD?Answer: Yes. If you need your currency to be printed on the invoice, please write an email to [email protected]. In 2 working-hours, we will create a special link for you to pay in any currencies. Otherwise, follow the normal steps: Add to Cart -- Checkout -- Select your currency to pay.
|