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GB 23200.3-2016 English PDF

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GB 23200.3-2016: Food safety national standard -- Methods for the determination of herbicide residues -- Part 3: Determination of cyclohexanone herbicides in food by liquid chromatography-mass spectrometry / mass spectrometry
Status: Valid

Standard ID	USD	BUY PDF	Lead-Days	Standard Title (Description)	Status
GB 23200.3-2016	399	Add to Cart	4 days	Food safety national standard -- Methods for the determination of herbicide residues -- Part 3: Determination of cyclohexanone herbicides in food by liquid chromatography-mass spectrometry / mass spectrometry	Valid

Similar standards

GB/T 38211 GB/T 18418 GB/T 18419 GB 23200.1 GB 23200.12 GB 23200.11

Basic data

Standard ID: GB 23200.3-2016 (GB23200.3-2016)
Description (Translated English): Food safety national standard -- Methods for the determination of herbicide residues -- Part 3: Determination of cyclohexanone herbicides in food by liquid chromatography-mass spectrometry / mass spectrometry
Sector / Industry: National Standard
Classification of Chinese Standard: G25
Word Count Estimation: 20,224
Date of Issue: 2016-12-18
Date of Implementation: 2017-06-18
Older Standard (superseded by this standard): SN/T 1737.3-2010
Regulation (derived from): State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No. 16 of 2016
Issuing agency(ies): National Health and Family Planning Commission of the People's Republic of China, State Food and Drug Administration

GB 23200.3-2016: Food safety national standard -- Methods for the determination of herbicide residues -- Part 3: Determination of cyclohexanone herbicides in food by liquid chromatography-mass spectrometry / 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.
Food safety national standard - Methods for the determination of herbicide residues - Part 3. Determination of cyclohexanone herbicides in food by liquid chromatography - mass spectrometry/mass spectrometry National Standards of People's Republic of China GB Instead of SN/T 1737.3-2010 National standards for food safety Method for determination of herbicide residue Part 3. Determination by liquid chromatography - mass spectrometry/mass spectrometry Residues of Cyclohexenone Herbicides in Food National food safety standards- Determination of cyclohexanediones herbicide residues in foods Liquid chromatography - mass spectrometry 2016-12-18 Release.2017-06-18 Implementation National Health and Family Planning Commission of the People 's Republic of China Issued by the Ministry of Agriculture of the People 's Republic of China State Administration of Food and Drug Administration

Foreword

This standard replaces SN/T 1737.3-2010 "Methods for the determination of herbicide residues Part 3. Determination by liquid chromatography-mass spectrometry Export of cyclohexene ketone herbicide residues ". Compared with SN/T 1737.3-2010, the main changes are as follows. - Standard text format is modified to national standard text format for food safety; - the name of the "import and export food" to "food"; - increase the "other food reference implementation" in the standard range. This standard replaced the previous version of the standard release. -SN/T 1737.3-2010. National standards for food safety Method for determination of herbicide residue Part 3. Determination of Cyclohexanone in Food by Liquid Chromatography - Mass Spectrometry/Mass Spectrometry Herbs Residue

1 Scope

This standard specifies the food in the pyranosone, grass grass, thiadenone, oxadiazone, alkenopyridine, butanone, trimethoprostenone, cyclophen Determination of Ketone Residue by Liquid Chromatography - Mass Spectrometry/Mass Spectrometry. This standard applies to rice, soybeans, pork, beef liver, chicken liver, milk, oranges, blueberries, spinach, onions, walnuts, tea Determination of the Residual Amount of Pyrrithione, Herbicide, Thiomethoxone, Cenotrocerone, Energeno, And confirmed that other food can refer to the implementation.

2 normative reference documents

The following documents are indispensable for the application of this document. For dated references, only the dated edition applies to this article Pieces. For undated references, the latest edition (including all modifications) applies to this document. GB 2763 National Standard for Food Safety - Maximum Residue Limit of Pesticides in Foodstuffs GB/T 6682 Analytical laboratory water specifications and test methods

3 principle

The residual cyclohexenone herbicides in the sample were extracted with acidic acetonitrile or acetonitrile, and the extract was treated with N-propyl ethylenediamine (PSA), octadecane (ODS) and graphitized carbon black were purified by liquid chromatography-mass spectrometry/mass spectrometry and quantified by external standard method.

4 reagents and materials

Unless otherwise specified, all reagents are of analytical grade and water is in accordance with the primary water specified in GB/T 6682. 4.1 Reagents 4.1.1 Acetonitrile (CH3CN). Chromatographically pure. 4.1.2 Acetic acid (CH3COOH) (99.5%). 4.1.3 Formic acid (HCOOH) (88.0%). 4.1.4 Sodium acetate (CH3COONa). 4.1.5 Sodium chloride (NaCl). 4.1.6 anhydrous magnesium sulfate (MgSO4). 650 ℃ burning 4 h, placed in the dryer to spare. 4.2 solution preparation 4.2.1 1% acetic acid acetonitrile solution. take 10 mL of acetic acid, add 990 mL of acetonitrile, mix. 4.2.2 60% acetonitrile aqueous solution. take 60 mL of acetonitrile, add 40 mL of water, mix. 4.2.3 Formic acid - Aqueous solution (0.2 999.8, V/V). Take 0.2 mL of formic acid, dissolve with water and dilute to 1000 mL. 4.3 standards 4.3.1 Cyclohexenone standards. Clethodim, CAS. 99129-21-2, purity ≥99%; pyranone (Tepraloxydim) CAS. 149979-41-9, purity ≥99%; thiadenone (Cycloxydim), CAS. 101205-02-1, purity ≥93.5%; Tralkoxydim, CAS. 87820-88-0, purity ≥93.5%; Alloxydim, CAS. 55634-91-8, purity ≥98%; Profoxydim, CAS. 139001-49-3, purity ≥98.5%; butanone (Butroxydim), CAS. 138164-12-2; Purity ≥99%; Sethoxydim CAS. 74051-80-2; Purity ≥99%. 4.4 standard solution preparation 4.4.1 Cyclohexenone Standard Reserve Solution. Accurately weigh the standard amount of cyclohexenone, dissolve with acetonitrile and set to 100 mL of brown Color container, the concentration of 100 μg/mL standard stock solution, the solution stored in dark. 4.4.2 mixed standard intermediate solution. accurate extraction of cyclohexene ketone standard stock solution of 2.5mL in 50mL brown volumetric flask, with acetonitrile Diluted to a concentration of 5.0 μg/mL mixed standard intermediate solution, the solution stored in dark. 4.4.3 Mixing standard working solution. Prepare the appropriate standard working solution with a blank sample matrix prior to use. 4.5 Materials 4.5.1 Graphitized Carbon Black Adsorbent. 120 μm to 400 μm. 4.5.2 N-propyl ethylenediamine (PSA) adsorbent. 40 μm to 100 μm. 4.5.3 Octadecylsilane (ODS) Bonded phase. 40 μm to 100 μm. 4.5.4 Water phase filter. 0.22 μm.

5 instruments and equipment

5.1 LC-MS/MS. ESI ionization source. 5.2 Electronic balance. 0.01 g and 0.0001 g. 5.3 Crusher. 5.4 Tissue crusher. 5.5 Centrifuge. 4 000 r/min. 5.6 vortex mixer. 5.7 nitrogen blowing instrument. 5.8 Homogenizer. 10 000 r/min. 5.9 screw cap polypropylene centrifuge tube. 50 mL, 15 mL. 5.10 glass with a plug centrifuge tube. 15 mL.

6 Preparation and storage of samples

6.1 Preparation of the sample 6.1.1 Oranges, blueberries, spinach, onions Take a representative sample of about 500 g (can not be washed with water), cut it, and then use the tissue crusher to process the sample into a slurry, The net container is sealed as a sample, marked and marked. 6.1.2 Soybean, rice, tea, walnut Approximately 500 g of representative sample, crushed and mixed with a pulverizer, packed in a clean container as a sample, sealed and marked. 6.1.3 pork, bovine liver, chicken liver Take a representative sample of about 500 g, chopped, with the tissue crusher will be fully mashed evenly, into the clean container as a sample, sealed And mark the mark. Note. The above sample sampling site according to GB 2763 Appendix A implementation. 6.2 Sample storage Soybeans, rice, tea, walnut and milk and other samples at 0 ℃ ~ 4 ℃ preservation; oranges, blueberries, spinach, onions, pork, Chicken liver and other samples stored at -18 ℃ below. During the operation of the sample preparation, the contamination of the sample or the change in the content of the residue should be prevented.

7 Analysis steps

7.1 Extraction 7.1.1 Soybean, rice, tea and walnut Weigh the sample 5 g (tea sample 2 g, accurate to 0.01 g) in 50 mL screw cap polypropylene centrifuge tube, add 10 mL of water, Vortex mixer for 30 min, placed 15 min. Add 3 g of anhydrous magnesium sulfate, 1 g of sodium chloride, 1 g of sodium acetate and 15 mL of 1% acetonitrile solution, The homogenizer was centrifuged at 10 000 r/min for 2 min and 4 000 r/min for 5 min. The supernatant was transferred to a 25 mL volumetric flask. Reuse 10 mL 1% acetic acid acetonitrile solution to extract once again, the combined extract in the same 25 mL volumetric flask, and acetonitrile volume to the scale, to be purified. 7.1.2 Pork, Bovine Liver, Chicken Liver, Milk, Oranges, Spinach and Onion Weigh the sample about 5 g (accurate to 0.01 g) in a 50 mL screw cap polypropylene centrifuge tube, add 5 mL of water, 3 g of anhydrous magnesium sulfate, 1 g Sodium chloride, 1 g of sodium acetate and 15 mL of 1% acetic acid in acetonitrile, homogenized at 10 000 r/min homogenized for 2 min, 4 000 r/min centrifuged 5 Min. The supernatant was transferred to a 25 mL volumetric flask. And then 10 mL 1% acetic acid acetonitrile solution repeated extraction time, combined extract in the same 25 mL Volumetric flask, and fixed to the scale with acetonitrile, to be purified. 7.1.3 Blueberry Weigh the sample about 5 g (accurate to 0.01 g) in a 50 mL screw cap polypropylene centrifuge tube, add 5 mL of water, 3 g of anhydrous magnesium sulfate, 1 g Sodium chloride, 1 g sodium acetate and 15 mL acetonitrile, homogenized at 10 000 r/min homogenization for 2 min and 4 000 r/min for 5 min. Will be on The supernatant was transferred to a 25 mL volumetric flask. And then 10 mL of acetonitrile repeated extraction time, combined extract in the same 25 mL volumetric flask, and acetonitrile Constant volume to scale, to be purified. 7.2 Purification 7.2.1 Soybeans, rice, walnuts, pork, beef liver, milk, onions Remove 8 mL of the above extract in a 15 mL screw cap polypropylene centrifuge tube, add 300 mg of anhydrous magnesium sulfate, 250 mg of PSA and 500 mg ODS, mixed on a vortex mixer for 2 min, and centrifuged at 4 000 r/min for 5 min. Accurately remove 5 mL of the wash solution in 15 mL glass Tube, by 60 ℃ nitrogen blowing machine after drying, with 60% acetonitrile aqueous solution and set the volume of 1.0 mL, 0.22 μm filter for liquid chromatography-mass spectrometry / Mass spectrometer. 7.2.2 Chicken liver, orange, spinach, blueberry, tea Remove 8 mL of the above extract in a 15 mL screw cap polypropylene centrifuge tube, add 300 mg of anhydrous magnesium sulfate, 250 mg PSA, 500 mg ODS And 10 mg of graphitized carbon black were mixed on a vortex mixer for 2 min and centrifuged at 4 000 r/min for 5 min. Accurately remove 5 mL of the purified solution at 15 mL Glass with a plug centrifuge tube, by 60 ℃ nitrogen blowing machine after drying, with 60% acetonitrile aqueous solution and volume 1.0 mL, 0.22 μm filter for liquid Determination by mass spectrometry/mass spectrometry/mass spectrometry. 7.3 Determination 7.3.1 Liquid Chromatographic Reference Conditions 7.3.1.1 Column. C18, 50 mm × 2.1 mm (id), particle size 1.7 μm, or equivalent; 7.3.1.2 Mobile phase. see gradient elution program Table 1; Table 1 gradient elution program table 7.3.1.3 Flow rate. 0.25 mL/min; 7.3.1.4 Column temperature. 30 ° C; 7.3.1.5 Injection volume. 5 μL; 7.3.2 Mass spectrometry reference conditions See Appendix A. 7.3.3 Liquid Chromatography - Mass Spectrometry/Mass Spectrometry Detection and Verification According to the content of the sample in the sample solution, the selected concentration and sample solution similar to the standard working solution. Standard working solution and sample solution The ketene response value should be within the linear range of the instrument. The standard working solution and sample solution were measured by volume injection. In the above liquid phase color The retention time of cyclohexene ketone was 2.83 min, 3.40 min, thiazolone 3.81 min, Oxaliplatin 3.89 min, olefinic acid 4.05 min, lettuceone 4.08 min, trimethylbenzenone 4.17 min, cycloasproxone 4.83 min. Cyclodextone Standards for Liquid Chromatography-Mass Spectrometry/Mass Spectrometry Multi-Reaction Monitoring Chromatograms are given in Appendix B, Figure B.1. In the above liquid chromatography-mass spectrometry conditions, the retention time of the material to be measured in the sample is different from that of the standard working solution. ± 2.5%, and the relative ion abundance of the test substance in the sample is compared with the relative ion abundance of the standard working solution, The allowable relative deviation does not exceed the range specified in Table 2, it can be determined that there is a corresponding analyte in the sample. Table 2 The maximum allowable deviation of relative ion abundance when qualitative confirmation Relative abundance (base) 50% 20% to 50% 10% to 20% ≤10% Allowable relative deviation ± 20% ± 25% ± 30% ± 50% 7.4 blank test In addition to the sample, according to the above steps. Time (min) formic acid aqueous solution (3.9),% acetonitrile,% 0.25 60 40 1.50 60 40 1.60 40 60 2.00 40 60 3.00 20 80 4.50 20 80 5.00 60 40 6.00 60 40

8 results are calculated and expressed

Use the LC-MS/MS chromatographic data processor or calculate the residual content of cyclohexenyl ketone in the sample according to formula (1). The calculation result is deductible value. MΑsi VCsiAi   (1) Where. Xi - The amount of cyclohexene ketone in the sample, in micrograms per kilogram (μg/kg); The peak area of cyclohexene ketone in sample solution; Csi - Concentration of cyclohexenyl ketone in standard working fluid in ng/ml (ng/mL); V - the final volume of the sample solution in milliliters (mL); Asi - the peak area of cyclohexene ketone in standard working fluid; M - the mass of the sample represented by the final sample, in grams (g). Note. The result of the calculation shall be deducted from the blank value. The result of the measurement shall be expressed as the arithmetic mean of the parallel measurement, and two valid digits shall be retained.

9 precision

9.1 The ratio of the absolute difference between the two independent determinations obtained under reproducibility and its arithmetic mean (percentage) shall be in accordance with Appendix D requirements. 9.2 The ratio of the absolute difference between the two independent determinations obtained under reproducibility and its arithmetic mean (percentage) shall be in accordance with Appendix E requirements. 10% limit and recovery rate 10.1 Quantitation limits The quantification limit of this method is 5 μg/kg. 10.2 Recovery rate The data for the concentration, recovery and precision of the sample are given in Appendix C.

Appendix A

(Informative) Mass spectrometry reference conditions Table A.1 Mass Spectrometry Reference Conditions Ion source ESI, positive mode Scanning mode multiple reaction monitoring MRM Source temperature 110 ℃ Solvent gas flow rate 550 L/hr, nitrogen The solvent temperature was 350 ° C Taper hole air flow 50 L/hr, nitrogen Collision gas pressure 3.30 × 10 - 3 mbar, argon, purity ≥ 99.999% Capillary voltage 3.0 KV Table A.2 Multi-reaction monitoring conditions Compound parent ion (M/z) Ion (M/z) Dwell time (S) Cone hole voltage (V) Collision energy (EV) Grass off 324.7 178.4 266.5 * 0.02 23 21 0.02 23 12 Thiadenone 326.4 180.2 0.02 20 20 280.3 * 0.02 20 13 Dilute pyridine 328.3 178.1 * 0.02 12 20 282.2 0.02 12 11 Trimethylbenzene 330.3 137.9 0.02 24 24 284.2 * 0.02 24 12 Pyranone 342.4 166.1 0.02 22 21 250.3 * 0.02 22 14 Oxadiazone 360.2 164.1 * 0.02 24 19 268.3 0.02 24 13 Butanone 400.4 138.1 0.02 28 23 354.3 * 0.02 28 15 Cyclohexanone 466.2 180.2 0.02 25 25 280.3 * 0.02 25 15 Note. The ions with "*" in Table A.2 are quantitative ions. Non-commercial notices. The reference mass spectrometry conditions listed in Appendix A are performed on a Waters Quattro Premier LC/MS, where the test type Is for reference only and does not involve commercial purposes and encourages standard users to attempt to use instruments of different manufacturers or models.

Appendix B

(Informative) Cyclohexenone Standards Multi - Reaction Monitoring Chromatograms Figure B.1 Cyclohexenone Standards Liquid Chromatography-Mass Spectrometry/Mass Spectrometry Multi-Reaction Monitoring Chromatogram

Appendix C

(Informative) Recovery and precision Table C.1 Data on the concentration, recovery and precision of the sample (%) Concentration (%) Concentration of sample compound concentration (μg/kg) Recovery range (%) Precision (%) Concentration (%) Concentration (%) Concentration (%) Concentration (% Pyranone 5 75.20 to 101.00 10.16 Pyrione 4 76.40 ~ 98.40 8.58 10 81.30 ~ 103.80 8.93 10 79.50 ~ 103.50 9.03 50 77.04 ~ 102.64 9.72 50 80.80 ~ 102.84 8.91 Herbs off 5 76.80 ~ 101.00 9.95 Herbs off 5 80.80 ~ 103.20 8.29 10 75.60 ~ 101.10 8.24 10 78.90 ~ 102.60 7.77 50 80.52 ~ 101.40 7.59 50 78.26 ~ 102.36 9.49 Thiabendone 5 76.4 ~ 102.20 9.73 Thiadenone 5 76.20 ~ 98.40 6.54 10 81.70 ~ 107.00 9.16 10 81.00 ~ 104.30 9.35 50 79.40 ~ 102.20 8.20 50 86.32 ~ 103.36 5.84 Oxadiazone 5 76.4 to 105.00 10.15 oxadiazone 5 83.20 to 109.40 9.23 10 75.90 ~ 94.10 6.76 10 80.60 ~ 104.80 10.02 50 73.24 ~ 94.58 9.73 50 80.44 ~ 100.32 8.26 Dilute pyridine 5 84.00 ~ 103.60 6.19 diltthlor 5 82.60 ~ 104.80 7.77 10 88.20 ~ 103.20 5.14 10 75.30 ~ 98.10 7.22 50 82.06 ~ 104.34 8.30 50 82.70 ~ 104.26 8.20 Table C.1 (continued) Butoxfen 5 83.12 ~ 105.60 6.19 Butanone 5 77.40 to 103.20 10.02 10 80.00 ~ 98.40 5.14 10 76.90 ~ 97.30 8.31 50 79.46 ~ 100.62 8.30 50 77.42 ~ 102.86 10.22 Trimesterone 5 78.60 ~ 102.20 8.20 Trimethoproxone 5 76.20 ~ 107.00 7.90 10 81.20 ~ 104.20 7.84 10 80.50 to 101.70 10.39 50 87.12 ~ 103.76 5.94 50 80.86 ~ 99.56 6.14 Cyclohexanone 5 82.20 to 104.20 8.47 Cyclohexanone 5 81.60 ~ 108.60 8.58 10 74.20 ~ 101.00 8.24 10 77.60 ~ 98.70 5.89 50 78.76 ~ 94.84 6.45 50 78.94 ~ 98.34 8.31 Pyrrione 5 74.60 ~ 103.80 9.82 Pyrrione 5 78.40 ~ 99.60 7.97 10 79.10 ~ 97.30 6.58 10 78.10 ~ 102.10 11.19 50 75.80 ~ 98.76 7.93 50 83.12 ~ 100.64 7.69 Herbs off 5 76.80 ~ 101.40 7.12 Herbs off 5 73.60 ~ 98.40 5.67 10 81.50 to 101.10 6.53 10 78.40 to 100.70 7.61 50 77.66 ~ 96.88 7.43 50 80.22 ~ 99.34 8.32 Thiabendone 5 76.40 ~ 108.60 10.22 Thiomethoxone 5 76.40 ~ 101.20 6.33 10 78.90 ~ 101.70 9.00 10 76.70 ~ 101.30 9.71 50 78.28 ~ 102.12 8.96 50 83.36 ~ 104.20 7.91 Table C.1 (continued) Oxadiazone 5 79.40 to 100.80 8.33 Oxadiazone 5 76.20 to 103.20 9.43 10 75.90 ~ 105.70 10.18 10 79.40 ~ 97.30 7.77 50 76.66 ~ 96.88 7.60 50 78.88 ~ 99.24 7.88 Dilute pyridine 5 77.20 ~ 103.60 8.87 diltthlor 5 75.80 ~ 106.40 10.24 10 76.40 ~ 104.70 10.47 10 78.50 ~ 103.50 9.25 50 79.52 ~ 101.46 7.74 50 78.86 ~ 97.00 6.68 Butroxydim ~ 5 74.40 99.40 76.00 5 8.34 butroxydim - 105.40 10.05 10 78.40 ~ 96.20 7.31 10 76.10 ~ 102.60 9.23 50 77.08 to 102.06 10.38 50 79.46 to 102.72 8.36 Trimethoproxone 5 74.20 to 103.40 9.66 Trimethylpenone 5 78.20 to 98.40 7.80 10 75.40 to 98.40 7.79 10 79.50 to 105.80 10.04 50 81.74 ~ 102.54 8.07 50 80.72 ~ 103.36 6.61 Cyclohexanone 5 77.40 ~ 103.80 9.48 Cyclohexanone 5 82.00 ~ 109.40 9.99 10 78.60 ~ 106.70 7.70 10 81.60 ~ 104.80 6.99 50 77.14 ~ 96.54 8.34 50 82.04 ~ 97.94 6.54 Pyrione 5 80.20 ~ 103.60 7.99 Spinach Pyranone 5 81.20 to 106.80 8.60 10 79.40 to 103.20 9.10 10 78.90 to 101.60 8.33 50 84.12 ~ 102.84 6.79 50 80.22 ~ 99.24 7.57 Table C.1 (continued) Grasses 5 77.40 ~ 103.60 8.87 Herbs off 5 80.40 ~ 104.80 9.47 10 79.50 to 103.30 8.75 10 76.20 to 103.50 9.12 50 82.90 ~ 104.62 7.50 50 8020 ~ 100.72 7.03 Thiadenone 5 82.20 ~ 105.40 8.45 Thiadenone 5 80.00 ~ 105.60 9.04 10 83.10 ~ 104.20 7.73 10 81.60 ~ 105.50 8.85 50 88.70 ~ 103.42 5.22 50 82.06 ~ 106.60 8.68 Oxadiazone 5 81.40 ~ 107.60 9.46 oxadiazone 5 82.60 ~ 100.00 7.17 10 81.60 ~ 105.40 8.16 10 84.00 ~ 105.70 7.59 50 84.70 ~ 101.94 6.71 50 83.20 ~ 108.06 6.88 Dilute pyridine 5 80.20 ~ 104.00 8.23 dilute pyridine 5 82.00 ~ 105.40 9.01 10 79.20 to 95.80 6.31 10 81.20 to 101.10 9.66 50 79.70 ~ 102.74 8.39 50 88.70 ~ 102.72 5.09 Butoxfen 5 77.60 ~ 105.60 10.55 Butanone 5 76.20 ~ 99.60 7.66 10 79.40 ~ 95.40 6.48 10 78.60 ~ 105.10 9.42 50 80.06 ~ 104.02 6.99 50 80.72 ~ 106.20 7.77 Trimesterone 5 83.20 to ......

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Answer: Upon your order, we will start to translate GB 23200.3-2016_English as soon as possible, and keep you informed of the progress. The lead time is typically 2 ~ 4 working days. The lengthier the document the longer the lead time.

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Question 3: Does the price include tax/VAT?

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