NY/T 1653-2008 Determination of mineral elements in vegetables, fruits and their products Inductively coupled plasma emission spectrometry NY/T1653-2008 standard download decompression password: www.bzxz.net
This standard specifies the determination method of phosphorus, calcium, magnesium, iron, manganese, copper, zinc, potassium, sodium and boron content in vegetables, fruits and their products by inductively coupled plasma emission spectrometry. This standard is applicable to the determination of phosphorus, calcium, magnesium, iron, manganese, copper, zinc, potassium, sodium and boron content in vegetables, fruits and their products.

ICS67.080.20
Agricultural Industry Standard of the People's Republic of China
NY/T1653—2008
Determination for mineral elements in vegetables, fruits and derived products by ICP-AES method2008-07-14 Issued
2008-08-10 Implementation
Issued by the Ministry of Agriculture of the People's Republic of China
Appendix A and Appendix B of this standard are informative appendices. This standard is proposed and managed by the Ministry of Agriculture of the People's Republic of China. NY/T1653—2008
Drafting units of this standard: Vegetable Quality Supervision, Inspection and Testing Center of the Ministry of Agriculture (Beijing), Institute of Agricultural Quality Standards and Testing Technology of the Chinese Academy of Agricultural Sciences.
Main drafters of this standard: Liu Zhongxiao, Yang Mao, Liu Su, Gao Ping. 1 Scope
Determination of mineral elements in vegetables, fruits and their products Inductively coupled plasma emission spectrometry
NY/T1653—2008
This standard specifies the method for determining the content of phosphorus, calcium, magnesium, iron, manganese, copper, zinc, potassium, sodium and boron in vegetables, fruits and their products by inductively coupled plasma emission spectrometry.
This standard is applicable to the determination of phosphorus, calcium, magnesium, iron, manganese, copper, zinc, potassium, sodium and boron in vegetables, fruits and their products. The linear range of this method is 0～500mg/L. The detection limit of this method is 0.001mg/L～0.171mg/L (see Appendix A, 1 for details). 2 Principle
After the sample is digested with acid and high temperature, it is excited in a plasma torch at a high temperature of 6000K～10000K. The element to be measured excites the light of the characteristic spectrum line, and its intensity is measured after spectroscopy.
3 Reagents
This method shall use at least confirmed high-purity reagents and first-grade water specified in GB/T6682. 3.1 Perchloric acid [HCIO, d~1.60g/cm]. 3.2 Nitric acid [HNO, d~1.42g/cm2].
3.3 Hydrogen peroxide p(H,Oz)=30%].
3.4 ​​Nitric acid solution Lg(HNOs)=5%: measure 50mL nitric acid (3.2) and dilute to 1000mL. 3.5 Nitric acid solution Lg(HNOs)=2%]: measure 20mL nitric acid (3.2) and dilute to 1000mL. 3.6 Mixed acid digestion solution [with (HNO+HCIO,)=4+1]: mix 4 parts of nitric acid (3.2) with 1 part of perchloric acid (3.1). 3.7 The mass concentration of each element standard stock solution is 1000 mg/L. 4 Instruments and equipment
4.1 Inductively coupled plasma emission spectrometer. 4.2 Microwave digestion instrument.
4.3 Analytical balance: sensitivity 0.01g, 0.0001g. 4.4 Tissue crusher.
4.5 Adjustable temperature electric heating plate.
4.6 Muffle furnace.
5 Sample preparation
5.1 Fruit and vegetable sauce products
Stir the sample evenly.
5.2 Fresh fruits and vegetables
Take the edible part of the fruit and vegetable sample, wash it with tap water and deionized water in turn, and gently wipe off the surface moisture with clean gauze. For grapes, hawthorns and other small individuals, several individuals can be randomly selected, chopped and mixed; for watermelons, Chinese cabbages and other large individuals, cut into 4 parts along the cross of their growth axis, take 2 diagonal parts, chop them and mix them thoroughly. Use the quartering method to take samples or directly put them into a tissue masher to make a homogenate. For samples with less juice, an equal amount of deionized water can be added according to a certain mass ratio. Put the homogenate in a polyethylene bottle and store it at -20℃ to -16℃; or use the quartering method to take samples and put them into an oven to dry at 65℃, grind them into dry powder and store them in a sealed container. 5.3 Canned and frozen foods
Pour all canned and thawed frozen samples into a tissue masher to make a homogenate, and put the homogenate sample into a polyethylene bottle and store it at -20℃ to -16℃.
6 Analysis steps
6.1 Preparation of test solution
6.1.1 Ashing method: Weigh 0.5g of uniform dry sample, accurate to 0.0001g, into 40mL porcelain, place on an adjustable temperature hot plate for complete carbonization, then transfer to a muffle furnace and ash at 550℃ for 4h. Take out and cool to room temperature, dissolve the residue with 5mL nitric acid solution (3.4), boil, transfer to a 50mL volumetric flask, make up to volume with nitric acid solution (3.4), mix and set aside. 6.1.2 Digestion method: Pipette 20mL of liquid sample, or weigh 20g, accurate to 0.01g; weigh 10g of fruit and vegetable sauce products or frozen and canned food homogenate, accurate to 0.01g; weigh 10g-20g of fresh fruit and vegetable sample homogenate, accurate to 0.01g; weigh 0.5g of uniform dry sample, accurate to 0.0001g, add 10.0mL of mixed acid digestion solution (3.6) in a 100mL beaker, cover with blood, place on the hot plate for digestion until white perchloric acid smoke appears and the digestion solution is clear. If the digestion solution is brown-black, add a few milliliters of mixed acid and continue heating and digestion until white perchloric acid smoke appears and the digestion solution is clear. After cooling, transfer to a 25mL or 50mL volumetric flask with nitric acid solution (3.5) to make up the volume, mix well and set aside. The above operation is a blank test. 6.1.3 Microwave digestion method: Weigh 0.1g~0.3g of uniform dry sample, accurate to 0.0001g, place in a Teflon dissolving cup, add 3mL~5mL nitric acid solution (3.2), pre-react overnight, add 0.5mL hydrogen peroxide (3.3), after the reaction is stable, cover the dissolving cover, place in a high-pressure tank, and then put it in a microwave dissolving device, and start dissolving the sample according to the set microwave dissolving program. After the sample is dissolved, cool to room temperature, dilute to 25mL with water, and shake well. Perform a blank test at the same time. 6.2 Preparation of standard working solution
Use nitric acid solution (3.4) as standard working solution 1. Prepare mixed standard working solution 2 and standard working solution 3 according to the content of each element in the sample to be tested. For the preparation of each element, refer to Appendix A2.6.3 Determination
6.3.1 Determination of standard working curve: Determine standard working solutions 1, 2, and 3 in turn to determine the standard working curve. 6.3.2 Sample determination: Determine the blank solution and the sample solution in turn. Clean the pipeline for 20s~30s before each injection. If the content of the element to be determined is greater than the highest point of the standard curve, it should be diluted before determination. 7 Result calculation
The content of the element to be determined in the sample is expressed as mass fraction w, and the value is expressed in milligrams per kilogram (mg/kg) or milligrams per liter (mg/L). It is calculated according to formula (1):
w(ep)xVxt..
Where:
β——mass concentration of the element in the solution to be determined, in milligrams per liter (mg/L); Po-mass concentration of the element in the blank solution, in milligrams per liter (mg/L); V is a constant volume, in milliliter (mL); t. dilution factor;
is the mass or volume of the sample, in grams (g) or milliliters (mL). NY/T1653—2008
The calculation result shall retain three significant figures. If fresh fruits and vegetables are tested after drying, the final calculation result shall be converted to the original natural state. 8 Precision
The absolute difference between two independent test results obtained under repeatability conditions shall not exceed 10% of the arithmetic mean of the two measured values, provided that the absolute difference is greater than 10% of the arithmetic mean of the two measured values ​​and does not exceed 5%. NY/T1653—2008
A.1 Detection limit
2 Preparation of mixed standard working curve
Appendix A
(Informative Appendix)
Table A1 of detection limit of each element and preparation of standard mixed solution
Detection limit of each element
Detection limit
2 Preparation table of standard mixed solution
Mass concentration of standard working solution 2
Mass concentration of standard working solution 3www.bzxz.net
Cooling gas
Appendix B
(Informative Appendix)
Reference conditions for instrumental determination
Reference conditions for instrumental determination
Auxiliary gas
Nebulizer
Pa/cm2
NY/T16532008
mL/min
Tip: This standard content only shows part of the intercepted content of the complete standard. If you need the complete standard, please go to the top to download the complete standard document for free.