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1.
This method is suitable for the determination of cyanide and total cyanide in soil
Second, the principle of the method
Isonicotinic acid- pyrazolone spectrophotometry
3.
Unless otherwise specified, analytical reagents conforming to national standards are used for analysis, and the experimental water is newly prepared distilled water or deionized water
(1) Tartaric acid solution: p(C 4 H 6 O 6 )=150g/L
Weigh 15.
(2) Zinc nitrate solution: p[Zn(NO 3 ) 2 ·6H 2 O=100g/L
Weigh 10.
(3) Phosphoric acid : p(H 3 PO 4 )=1.
(4) Hydrochloric acid : p(HCL)=1.
(5) Hydrochloric acid solution: c(HCL)=1mol/L
Measure 83 mL of hydrochloric acid and slowly inject it into the experimental water, let it cool and dilute to 1000 mL
(6) Stannous chloride solution: p(SnCl·2H 2 O)=50g/L
Weigh 5.
(7) Copper sulfate solution: p(CuSO 4 ·5H 2 O)=200g/L
Weigh 200g of copper sulfate pentahydrate and dissolve it in experimental water, dilute to 1000mL, and shake it up
.
(8) Oxygen sodium oxide solution: p(NaOH)=100g/L
.
Weigh 100g of sodium hydroxide and dissolve it in experimental water, dilute to 1000mL, shake well, and store in a polyethylene container
.
(9) Sodium hydroxide solution: p(NaOH)=20g/L
.
Weigh 20.
0 g of sodium hydroxide and dissolve it in experimental water, dilute to 1000 mL, shake well, and store in a polyethylene container
.
(10) Sodium hydroxide solution: p(NaOH)=10g/L
.
Weigh 10.
0 g of sodium hydroxide and dissolve it in experimental water, dilute to 1000 mL, shake well, and store in a polyethylene container
.
(11) Sodium hydroxide solution: p(NaOH)=1g/L
.
Weigh 1g of sodium hydroxide and dissolve it in experimental water, dilute to 1000mL, shake well, and store in a polyethylene container
.
(12) Chloramine T solution: p(C 7 H 7 ClNNaO 2 S·3H 2 O)=10 g/L
.
Weigh 1.
0 g of chloramine T and dissolve it in experimental water, dilute to 100 mL, shake well, store in a brown bottle, and prepare it immediately before use
.
(13) Phosphate buffer solution: pH=7
.
Weigh 34.
0 g of anhydrous potassium dihydrogen phosphate (KH 2 PO 4 ) and 35.
5 g of anhydrous disodium hydrogen phosphate (Na 2 HPO 4 ), dissolve in experimental water, dilute to 1000 mL, and shake well
.
(14) Isonicotinic acid-pyrazolone color developer
.
① Isonicotinic acid solution
.
Weigh 1.
5g of isonicotinic acid (C 6 H 6 NO 2 ) and dissolve it in 25mL of 20g/L sodium hydroxide solution, dilute with water and make the volume to 100mL
.
②Pyrazolinone solution
.
Weigh 0.
25g of pyrazolone (3-methyl-1-phenyl-5-pyrazolone, C 10 H 10 ON 2 ) and dissolve it in 20 mL of N,N-dimethylformamide [HCON(CH 3 ) 2 ]
.
③Isonicotinic acid-pyrazolone solution
Mix the above-mentioned pyrazolone solution and isonicotinic acid solution in a volume ratio of 1:5, and prepare them immediately before use
.
Note: If isonicotinic acid is prepared into a solution, if it is obviously light yellow, the blank value is increased, and it can be filtered
.
In the experiment, the colorless N,N-dimethylformamide is suitable
.
(15) Cyanide standard solution: p(CN)=100ug/mL
.
Purchase certified reference materials or weigh the corresponding solid cyanide to prepare
.
(16) Cyanide standard use solution: p(CN-)=0.
500ug/mL
.
Draw 5.
00mL of the above cyanide standard solution in a 1000mL brown volumetric flask, dilute to the mark with 1g/L sodium hydroxide solution, spread it evenly, and prepare it immediately before use
.
Related links: Soil mechanical composition density meter method (6)