GB/T 5009.112-2003 Determination of quinalphos residues in rice and citrus fruits

This standard specifies the determination of quinalphos in rice and citrus by gas chromatography. This standard is applicable to the determination of quinalphos residues in rice and citrus. The detection limit of this standard: quinalphos is 5×10 GB/T 5009.112-2003 Determination of quinalphos residues in rice and citrus GB/T5009.112-2003 Standard download decompression password: www.bzxz.net

ICS 67.040
National Standard of the People's Republic of China
GR/T5009.112--2003
Replaces GB{4520.6-14
Determination of amalphns residues in rice and orangesbzxz.net
Published on August 1, 2003
Ministry of Health of the People's Republic of China
Standardization Administration of the People's Republic of China
Implemented on January 1, 2004
GB/T 5009.112—2003
This standard replaces GB/T14929.6-1994 Method for determination of phosphorus residues in rice and citrus fruits 3. Compared with GB/T14929.6-1991, this standard has the following main modifications: The Chinese name of the standard has been revised, and the Chinese name of the standard has been changed to "Determination of phosphorus residues in rice and citrus fruits 3" CB/T20001.4-20001 Standard Method for determination of phosphorus residues in rice and citrus fruits Part 4: Chemical analysis method The structure of the source standard has been revised.
This standard is proposed and registered by the Ministry of Health of the People's Republic of China. The drafting unit of this standard is: Coal Research Institute of Jiangsu Academy of Agricultural Sciences. The original standard was first issued in 1994, and this standard is the first revision.
1 Scope
Determination of quinalphos residues in rice and citrus This standard specifies the rapid determination of quinalphos residues in rice and citrus using gas bridge chromatography. This standard is applicable to the determination of residual sulfur groups in rice and wheat. GB/T 5009.112-2003
This standard detects: the accuracy is 5×10-°g, the oxygen content is 2.5×10-g, and the detection validity of these test groups is 6.03g/k2. Principle
The mixed material is prepared by mixing with polyelectrolyte and washing with a mixed agent. After determination, it is determined by FPLGC. 3. 1 Reheat with acetone, 3.2 Reheat with 1% thioesterase, 3.3 No disulphide, 3.2091. Sodium dithioester
3.5 Silica gel (activated at 650°C for 4h~5h.3% water deactivated) 3.6 Quinalphos, purity 99.5%. 4. Fast instrument
41 Phase chromatograph head tip furnace photometric detector (iodine-filter). 4. 2 New grain sugar machine.
4.3 Two powder weak.
Year. 4 Vibrator,
4.5 Tissue sequencer,
4.6 Rate converter.
4.7 Mass radiator, 100μ.
4.8 Full instrument case Glass chromatography, separation bucket, container, true orang flask. 5 Analytical steps
5.1 Sample extraction
Weigh the maximum 50.00 (whole powder) or nuclear effect (slurry) or 0.00 () into a 2m Erlenmeyer flask, mix with half (1-1.00) of solvent, use 10m according to the need for 50m, and filter with a sand filter. In the remaining parts, the filters are combined and filtered. 5.2 Purification
The whole aspirated stream from the upper part was transferred to a flask. The water was dehydrated by adding 10 mL of 2 mL of phenol and then transferred to a bottom flask. The water was concentrated under reduced pressure in water. 3 mL of phenol was removed. The 10 mL of phenol was removed by adding 10 mL of phenol. The 10 mL of phenol was removed by adding 10 mL of phenol. The 10 mL of phenol was removed by adding 10 mL of phenol. The 10 mL of phenol was removed by adding 10 mL of phenol. The 10 mL of phenol was removed by adding 10 mL of phenol. The 10 mL of phenol was removed by adding 10 mL of phenol. The 10 mL of phenol was removed by adding 10 mL of phenol. The 10 mL of phenol was removed by adding 10 mL of phenol. 5009.112—2003
5.3.2 Temperature: Column temperature 230%, injection port temperature 255℃, measuring end temperature 250℃. 5.3.3 Gas flow: carrier gas (hydrogen) 50nl./min, hydrogen 65mlmi1, air 30ml./min.5.3.4 Retention time
Under the above conditions, the retention time of chlorpyrifos is 3min4s, and the retention time of chlorpyrifos is 4min5s. 5.4 Determination
Qualitative determination by external standard method. Prepare 2×10-, 6×10-8×10-, 1G-*g/uL standard gas with chlorpyrifos and chlorpyrifos, inject 2uL, and measure the quotient. Take the peak height as the pseudo coordinate and the standard quantity as the offset coordinate, draw the work practice, according to the peak quotient of the sample (area> research quantity.
6 Result calculation
Calculate according to formula F:
Neutral phosphorus residual content of the sample, the unit is grams per kg): B-. The peak height of the measured sample is equivalent to the content in micrograms (g): The fixed volume before injection, the unit is liter (ml)4
Injection volume, the unit is magnetic opening ();
Trial selection, the unit is grams ()
Proof, cite the estimated calculation of the full code wine salt, will formula. ◆Iodine content (m/g) = flour content × precision (%) - the absolute difference between the two independent test results obtained under the conditions of hydrogen and iodine retention shall not exceed 10% of the standard. Other chromatographic factors of chlorpyrifos and chlorpyrifos: blank control chromatographic environment, high material, 1: bed and figure
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