GB/T 14550-2003 Determination of 666 and DDT in soil by gas chromatography
Some standard content:
n 13.080
National Standard of the People's Republic of China
GB/T14550—2003
Replaces G13/45501993
Method of gas chromatographic for determination of JHCandDDT in soil
Published on 2003-11-10
National Quality Supervision, Inspection and Quarantine Administration of the People's Republic of China
Implemented on 2004-04-01
GB/T 14550—2003
This standard is a replacement for GB/T1455U·19933 soil quality gas chromatography method for the following content
determination of hexachlorobenzene and titration ||tt| ... The main authors of this standard are Huang Zhongzhong, Liu Weicheng, Huang Yongchun, Gan Jizhi, Mai Guangxi, Xiang Xuming, Li Lengyang and Zhang Kehu. 1
1 Scope
Determination of 666 and DDT in soil
Gas chromatography
This standard specifies the determination method of 666 and DDT in soil. This standard applies to the analysis of the amount of organic ammonia in soil. 2 Normative references
CB/T1455D—2003
The following documents are used as references in this standard. The outdated documents, their amendments (including errata or revisions) are not applicable to this standard. However, the latest versions of these documents shall be used according to the agreement or agreement of this standard. For the documents with the date indicated, the latest version shall apply to this standard. G1T173321S98 Determination of multiple residues of organic oxygen and pyrethroids in food NY Agricultural soil environmental quality testing technology specification
3 Principle
Analysis of pesticide residues on the cooking station using organic extraction, liquid-liquid separation and carbonic acid chromatography purification of the remaining ten antibodies, using electrophoretic filter ECI detection according to the chromatographic selection to ensure qualitative, external standard rapid quantitative 1 Reagents and materials
4.1 Gas cut-off: Report gas (N,) purity 99.S9%. 4.2 Standard sample and soil purification materials. 1. Soil sample separation. All reagents used shall be fresh and absolute unless otherwise specified. Water shall be dry water.
4.2.1 Pesticide standard products:
& BH.A, HH, Y BHC, n-BHC, PP'-II, IFP, P.'-DDT, purity UX.O&-CO.
4.2.1.1 Preparation of pesticide standard solution (4.2.2): 19 mg per ml (accurate to ±0.11). First dissolve 3IIC in 10 ml of octane or n-hexane. Dilute to the mark in a volumetric flask. 4.2.1.2 Prepare the standard intermediate solution. Use a pipette to take eight pesticide standard drops respectively, transfer them to a 105L volumetric tank, and dilute them with isobutylene or hexane until the volume ratio of the eight prepared solutions is: Vc[VauxV,m+Vse+VeP-tceVa\lnVe3oeVr-mr=1:1:3.5:13.531 (applicable to filling in) 4.2.1.3 Prepare the pesticide standard working tank solution: According to the sensitivity and linearity requirements of the detector, use isobutylene or hexane to dilute the intermediate standard solution to prepare several standard solutions with different concentrations. Store at 4°C. 4.2.2F octane H.
4.2.3 C,H Manli 57--6ST year heat 4.2.4 Petroleum fermentation: 50℃~!0℃:, take. 4.2.5 Ketone (CHCCCII).
4.2. 6 Rice (C,II, , high-grade pure.
4.2.7 Concentrated acid (H, S,): high-grade ton:
4.2.8 Anhydrous sodium sulfate (NmSO1): baked in 33Y oven for 4h. Modify the detector for standby. GB/T14550-2003
4.2.9 Sodium sulfate solution: 20g/.
4.2.10 Silica gel: agent
5 Collector
5.1 Grease detector (case detector).
5.2 Rotary heat treatment.
5.3 Thinner,
5.4 Lead steel.
5.5 Centrifuge,
5.6 Calibrator Im; Sample bottle (glass ground mouth bottle), 300 mL separatory funnel, =0Cml. Conical flask, 10tml. Volumetric flask, 350 mL flat bottom flask, 25mL, 50mL, 00mL volumetric flask, 5.7 microdisc syringe.
5.B Gas chromatograph: with electron capture detector [\i radioactive source, 6 Samples
6.1 Sample properties
6.1.1 Sample type: soil,
6.1.2 Sample requirements: body,
6.1.3 Sample stability: 866 in 1 sample, chemical pressure compensation, 6.2. Sample requirements and storage methods
6.2. 1. The samples shall be collected in accordance with the relevant provisions of NY/T395. After collection, the samples shall be mixed thoroughly and stored in a freezer for later use after 50 days.
6.2.2 Sample storage: The samples shall be separated as soon as possible after collection: If not analyzed, they can be stored in a freezer at 18℃. 7. Analysis steps
7.1 Extraction
Accurately take 20.0 mL of soil from a small amount of water, add 4 mL of water, mix thoroughly, transfer to filter paper, cover with a piece of paper, and store in a freezer. 10CraT. No wake-up (11> 30mL of sample + 12, then heat extract at 75℃~9℃ for 4h, reflux 1-6 times each time, after cooling, transfer the collected liquid into a 300mL separatory funnel. Rinse the extractor flask with 10ml of stone once, and divide the washing liquid into the funnel. 10Cm of sodium monohydrate can be pressed, shake for 1m, let stand for 3 minutes, and then discard the original water solution in the oil extraction hoop for purification, 7.2 Purification
7.2. 1 bag of purification method (method: use 100% biological products, add 1/3 of the volume of concentrated sulfuric acid in the oil extract, select 1m. After placing in the room, the general standard is: during the purification process with concentrated acid, it is necessary to stop the heat before the explosion, add concentrated sulfuric acid slowly, and then release the gas in a relatively small amount), repeat the above steps several times, until the interface of the added extract is clear and obvious: then add about half of the volume of basic acid solution to the aldehyde extract and shake for more than ten minutes. After the layers are separated, the water layer is discarded. Repeat this process until the extract becomes neutral (one or more times). Remove the molten oil from the extract and pass it through a simple flow-through micro-channel with a small amount of anhydrous sodium bicarbonate. Concentrate the extract to 5 mL using a vortex benzene technique. Make up to volume and use it for gas chromatography determination. 7.2.2 Column purification method (F method): Follow the purification steps in (R/T17232-19446.2): 7.3 Gas chromatography determination 7.3.1 Determination case A 7.3.1.1 Column GB/174550--2003 a) Isolation, 2.0 m3/2 mm3, d) Fill with Chrotaosorb wAW-DMCS.~-1 carrier containing 15% UV:7i1.95% QF-1.
h) Glass end: 2.0m×2m(id filled with 1.5%0V17+1.5OV-211rarbWAW-DMC5HP80day--102cell.
7.3.1,2 Temperature chamber 13%~20℃ Vaporization chamber 220Detector 2--00℃.7.3.1.3 Gas-liquid velocity; oxygen (N,>5mr1./mi~7)ml/m1.7.3.1.4 Detector: Electron capture detector (ECD).7. 3.2 to each B
7.3.2. Note: 6 elastic-group to F-[,3rm×.25(id]: 7.3.2.2 Temperature, temperature using the rent sequence external temperature pressure type? Discharge: /260 20 2 28 ℃, recommended 220 standard media (ECD320 ℃. 15t
7.3.2.3 Volume flow rate, gas 1.5mL/ain 3y. More than mL/ma7.3.3 In gas chromatograph, the use of agricultural standard samples in the conditions of standard push product injection volume and sincere push volume alternate, standard full expansion of the response value close to the test item should be Bo, when a standard column injection twice, the relative deviation of the peak height (peak area) is less than 7%, that is, recognized In order to achieve the desired state, the standard sample and the test sample should be properly sampled and analyzed in the actual determination. 7.3.4 Sampling
7.3.4.1 Sampling method: syringe push-pull.
7.3.4.2 Sampling
7.3.5 Chromatogram
7.3.5.1 Chromatogram
Figure 1 adopts semi-fine analysis
7.3.5.2 Qualitative analysis
7.3.5.2.1 The chromatogram of the following: QC, 3HI3HC, 6-KHP, P'-1F,, PT, P PDDD, H. 7.3.5.2.2 To test the possible situation, adopt double scan qualitative analysis, use a 1.0V171.95% chromatograph with a 2.0V/cm2/10mc-HPA column, and perform confirmation test. The chromatographic analysis can confirm the concentration of hexachlorobenzene and the concentration of impurities.
7.3.5.3 Quantitative analysis
7.3.5.3.1 Gas chromatographic analysis
Take 1 mixed standard solution and inject it into the gas chromatographic scan. Record the peak time (or peak area) of the chromatogram, then absorb 1 sample and inject it into the gas chromatogram, record the peak time and peak area (peak area) of the chromatogram, and quickly return the peak area (or peak area) of the chromatogram to determine the quantity and quantity.
7.3.5. 3. 2 Calculation
Wu Zhong,
X-EYXl(S2V
V,XH,IS.IXm
The residual quantity in this volume is in grams (m): The standard allowable flow rate of the component in the table is in microliters per minute (uR/mT.): A standard sample injection volume, in microliters (μL): A sample volume is in the final volume (mL): V: Sample injection volume. In liters)3
GB/T 1455G-- 2003
A clinical solution, the component reported the longitudinal peak area m) H(S.-
Detailed rate of drop component I about the height (mm or peak length mm) called the appropriate single use grams!
2.. - k..
S-RJIG:
\-[TD:
S.-- . -..
Figure 1 Gas chromatogram of 666 and alcohol
Figure 2 Gas chromatogram of 666 and alcohol
B Representation of results
E.1 Qualitative results
CB/T14555—2003
The number and name of each component in the color of the non-standard product of the standard non-standard product
8,2 The result
B,2.1 The method of containing the world
The weight of each component is calculated. It is expressed in g/. Precision
Coefficient of variation %), 2.08~.3.1%. See Table 1.1. 2.3 Accuracy
Recovery of spiked substance: 9.2. See Table.
8,2.4 Limit of detection
Initial detection varies with concentration, 0,5×--mg/x--4,8×9-mg/k. Table A, 3.G/T 14550—2003
The precision of the method shall be based on Table A.1,
Agricultural name
i-KSHK:
\-131F:
Appendix A
Informative Appendix)
Summary of the method, accuracy and detection limit Table 4. 1 Precision
Specification energy limit g/kg?
..C2c6
.. 2X.
c. lix: n
Variation effect V)
Conditions: For actual use, it is necessary to do it when the actual collection is rich. In the test room, the allowable error is 13, 72, .2. 1: 6, 63, tt||. The soil is 23, 1, 24, 12. The accuracy of A.2 formula is shown in Table 4.2.
Pesticide name
(1. 1-1s1
Table A2 Method release
Degree (bug:kg)
G, 200 c
.non tt
Note: Collaborative experiment: Each company conducts 5 repeated tests on each of you. A.3 Method detection limit see Table A.3, minimum detection daily concentration see formula (A, 1. Table A.3 Detection limit soil filling
Drug name
FP-IHE
Method minimum detection concentration (mp/ks)
is small test herb/
3.73×1c#
1. 18x13=s
0, 75×1\
7.56×1c-
5. 57×.0-1:
1,e×l-
GB/T14550—2003
Confirmed spiked recovery rate)/(5%
k test pressure/mR.kz)
0.49×1n4
C. J3 ×IJ-
:9nx n,
4.87×10-1
Ken small detection amount (g text report agreed instrument volume (L) group this secret city English selection volume text sample ()
....-( A.1)Year position is for liter I)3
GB/T 1455G-- 2003
One-dimensional solution, component reported drug longitudinal n real peak Li area m) H(S.-
Detailed this rate of drop formula component I about the height (mm or peak length mm) called Xiang quality suitable single use is grams!
2.. - k..
S-RJIG:
\-[TD:
S.-- . -..
Figure 1 Gas chromatogram of 666 and alcohol
Figure 2 Gas chromatogram of 666 and alcohol
B Result representation
E.1 Qualitative results
CB/T14555—2003
The number and name of each component in the standard non-promoted product of the color noxious substance
8,2 The determination of the country with the fruit
B,2.1 The method of containing the world
The weight of each component was calculated. 3.3.5.2 The calculated value of each component is expressed in g/. Precision
Coefficient of variation (%), 2.08~.3.1%. See Table 1.1. 2.3 Accuracy
Recovery rate of spiked: 9.2. See Table.
8,2.4 Detection limit
Initial detection with concentration, 0,5×--mg/x--4,8×9-mg/k. Purchase Table A, 3.G/T 14550—2003
The precision of the method shall be based on Table A.1,
Name of agricultural products
i-KSHK:
\-131F:
Appendix A
Informative Appendix)
Abstract of the method, accuracy and detection limit Table 4. 1 Precision
Specification Energy limit g/kg?
..C2c6
.. 2X.
c. lix: n
Variation effect V)
Conditions: The actual test is firm, and the actual test is required to be done when the test is complete. In the test room, the allowable error is 13, 72, .2. 1: 6, 63, tt||. The soil is 23, 1, 24, 12. The accuracy of A.2 formula is shown in Table 4.2.
Pesticide name
(1. 1-1s1
Table A2 Method release
Degree (bug:kg)
G, 200 c
.non tt
Note: Collaborative experiment: Each company conducts 5 repeated tests on each of you. A.3 Method detection limit see Table A.3, minimum detection daily concentration see formula (A, 1. Table A.3 Detection limit soil filling
Drug name
FP-IHE
Method minimum detection concentration (mp/ks)
is small test herb/
3.73×1c#
1. 18x13=s
0, 75×1\
7.56×1c-
5. 57×.0-1:
1,e×l-
GB/T14550—2003
Confirmed spiked recovery rate)/(5%
k test pressure/mR.kz)
0.49×1n4
C. J3 ×IJ-
:9nx n,
4.87×10-1
Ken small detection amount (g text report agreed instrument volume (L) group this secret city English selection volume text sample ()
....-( A.1)Year position is for liter I)3
GB/T 1455G-- 2003
One-dimensional solution, component reported drug longitudinal n real peak Li area m) H(S.-
Detailed this rate of drop formula component I about the height (mm or peak length mm) called Xiang quality suitable single use is grams!
2.. - k..
S-RJIG:
\-[TD:
S.-- . -..
Figure 1 Gas chromatogram of 666 and alcohol
Figure 2 Gas chromatogram of 666 and alcohol
B Result representation
E.1 Qualitative results
CB/T14555—2003
The number and name of each component in the standard non-promoted product of the color noxious substance
8,2 The determination of the country with the fruitwww.bzxz.net
B,2.1 The method of containing the world
The weight of each component was calculated. 3.3.5.2 The calculated value of each component is expressed in g/. Precision
Coefficient of variation (%), 2.08~.3.1%. See Table 1.1. 2.3 Accuracy
Recovery rate of spiked: 9.2. See Table.
8,2.4 Detection limit
Initial detection with concentration, 0,5×--mg/x--4,8×9-mg/k. Purchase Table A, 3.G/T 14550—2003
The precision of the method shall be based on Table A.1,
Name of agricultural products
i-KSHK:
\-131F:
Appendix A
Informative Appendix)
Abstract of the method, accuracy and detection limit Table 4. 1 Precision
Specification Energy limit g/kg?
..C2c6
.. 2X.
c. lix: n
Variation effect V)
Conditions: The actual test is firm, and the actual test is required to be done when the test is complete. In the test room, the allowable error is 13, 72, .2. 1: 6, 63, tt||. The soil is 23, 1, 24, 12. The accuracy of A.2 formula is shown in Table 4.2.
Pesticide name
(1. 1-1s1
Table A2 Method release
Degree (bug:kg)
G, 200 c
.non tt
Note: Collaborative experiment: Each company conducts 5 repeated tests on each of you. A.3 Method detection limit see Table A.3, minimum detection daily concentration see formula (A, 1. Table A.3 Detection limit soil filling
Drug name
FP-IHE
Method minimum detection concentration (mp/ks)
is small test herb/
3.73×1c#
1. 18x13=s
0, 75×1\
7.56×1c-
5. 57×.0-1:
1,e×l-
GB/T14550—2003
Confirmed spiked recovery rate)/(5%
k test pressure/mR.kz)
0.49×1n4
C. J3 ×IJ-
:9nx n,
4.87×10-1
Ken small detection amount (g text report agreed instrument volume (L) group this secret city English selection volume text sample ()
....-( A.1)
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