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肥料研究報告 第7号 （2014）

Contents

1. Table 4 1 Statistical analysis of collaborative study results for melamine No of labs Mean s RSD s amp RSD 8 Sample 1 3 3 3 HorRat p q Calcium cyanamide 1 9 2 2 83 0 04 1 4 0 12 4 3 1 27 Calcium cyanamide 2 10 1 0 391 0 003 0 8 0 023 5 8 1 25 PAAU 9 2 0 845 0 019 22 0 036 42 10 containing calcium cyanamide Compound fertilizer 11 0 0 198 0 005 2 6 0 012 6 2 1 22 Amm
2. 0 Table 1 Homogeneity test results Saige No Mean s RSD Sbb son RSDow F Value sample 96 26 96 76 a 1 10 0 8 62 0 19 2 3 0 12 0 23 2 6 1 72 b 10 0 12 51 0 16 1 3 0 06 0 17 1 4 1 24 c 12 10 0 247 8 4 46 1 8 1 0 4 6 1 8 1 11 d 10 0 245 6 5 28 2 1 0 5 5 3 9 1 02 e 1 10 0 1 38 0 02 1 1 0 01 0 02 1 4 2 33 Tus 10 0 2 85 0 04 1 5 0 0 04 1 5 0 29 1 The number of samples used for analysis The number of outliers 2 Grand mean value n The number of samples used for analysis X The number of repetition times 2 3 Mass fraction 4 Standard deviation of repeatability 5 Relative standard deviation of repeatability 6
3. 50 24 Vol 7 2014 i 2 UL SUMIGRAPH NC 220F 3 1 Cochran 2 X10 9 Table 2 RSD
4. 25 7 2014 12 EA 7 2014 H X lt gt 1 LC MS MS
5. FAMIC 2006 6 ISO IEC 17043 JIS Q 17043 2013
6. 124 Vol 7 2014 2 1 RS 12 2 NP 6 3 AS ONE AS 01 4 APB 620 1 JIS K8617 EED IV JIS K8995 ire se LAE 2 S SiO 40 S Si02 25 S SiO 10 S
7. 16 Vol 7 2014 Table 3 4 Individual result of cyanuric acid mass Lab Calcium Calcium Tone wd ere Compound Ammonium ID cyanamide 1 cyanamide 2 POUR apum fertilizer sulfate cyanamide A 1 06 1 14 0 398 0 417 0 130 0 124 0 688 0 720 0 0375 0 0367 B 1 03 0 971 0 359 0 342 0 0807 0 0835 0 84 0 827 0 0415 0 0408 C 1 24 1 28 0 397 0 433 0 0965 0 102 0 846 0 852 0 0336 0 0330 D 123 1 21 0 408 0 411 0 122 0 119 0 776 0 818 0 0530 0 0502 E 1 25 1 07 0 335 0 391 0 104 0 100 0 831 0 665 0 0359 0 0345 F 117 1 21 0 383 0 360 0 0935 0 0892 0 819 0 750 0 0287 0 0294 G 1 03 99779 0 241 0 252 0 0454 0 0486 0 740 0 744 0 0295 0 0278 H 121 1 23 0 412 0 412 0 110 0 107 0 831 0 818 0 0363 0 0320 I 1 10 1 19 0 405 0 409 0 105 0 108 0 827 0 820 0 0378 0 0414 J 1 09 1 10 0 395 0 416 0 107 0 102 0 744 0 735 0 0337 0 0347 K 03928 0 541 0 350 0 360 0 0854 70 0422 0 710 0 769 0 0284 0 0303 1 Laboratory identification 2 Outlier of Cochran 4 Unexpected value deviated from a protocol 3
8. eT T 02 S SiO gt 60 46 11 3 4 1 35 15 Median 35 18 88 NIQR 0 55 HSD 0 59 2006 2012 NIQR 0 48 0 87 HSD 0 53 0 60 gt 3 one 2 1
9. 1 8 1 8 gum Quantity of cadmium uptake Sludge fertilizer application plot AP 1 6 1 6 E EN N L 1 Quantity of cadmium bisque plot SP M o Cadmium Concentration St andard plot SP Quantity of cadmium uptake mg plot z a 2 ob E g 1 0 1 0 S 0 8 0 8 9 g o 0 6 0 6 O g 0 4 0 4 g S 0 2 02 9 0 0 0 0 Carrot Spinach Spinach Qing geng cai Turnip Spinach Carrot Spinach Carrot Rootand leaf Edible portion Edible portion Edible portion Root and leaf Edible portion Root and leaf Edible portion Root and leaf 2009 2009 2010 2010 2011 2011 2012 2012 2013 Summer Winter Summer Winter Summer Winter Summer Winter Summer Fig 6 Absorption and the amount of cadmium concentration of each crops in 2009 2013 The error bar indicating the standard deviation 61 Year 2009 2009
10. 5 7 NIQR NIQR W Fe 0 240 966 NIOR 0 013 5 4 W Fe HorRat 1 09 AOAC OMA 9 1 0 1 4 6 W Fe
11. ISO IEC 17025 2005 JIS Q 17025 2005 FAMIC A FAMIC A 10 B FAMIC B 10 C FAMIC C 12 A B C amp 3 i 9 D ISO Guide 34 2009 JIS Q 0034 2012 S ISO Guide 35 2006 JIS Q 0035 2008 ISO Guide 31 2000 JIS Q 0031 2002 ZZ CB 2013
12. 0 3 1 2 X 10 Table 1 F F 9 10 0 05 ie 39 Table 1 Homogeneity test results of for soluble silicic acid 2 4 5 6 7 8 No of Mean Sr RSD S bb Sbar RSDb a Sampl ee sample s 9 s sy Value 9 10 Phosphate fertilizer mixture 1 10 0 24
13. 84 Vol 7 2014 6 C MgO 129 116 9 ICP 4 EDTA 3 6 6 19 Median 6 18 86 NIQR 0 13 HSD 0 19 9 12 11 ICP 1 1CP 5
14. Ey 2 1 1 CX JIS 2 Fe 0 01 967 10 Fe 0 001 1 2 1 Z 2310 2 ADVA
15. E 2 3 3 LC MS MS Fig 1
16. 1992 W Mo E 1 JIS 2 L Mo 0 002 54 34 alli 2 1 UVmini 1240 2
17. 10 0 v 2 1 2 1 20 g L 20 g L 1 23 L
18. 106 Vol 7 2014 3 a b c d 1 A B C 1 E 2A 2B 2C E A B 207 A 247 a FAMIC
19. 4 2013 TERR ISO Guide 35 2006 JIS Q 0035 2008 IEEE Alt fe EDH LAS TEE DER T9 Tz 2014 4 wo RERE F 1 23 fit E A E E IRRD T EE E v gv B ie ale Be iE SIR dre D ROE D BRIT UE OS HEE EXE PE wo 4 e
20. Vol 7 2014 2 2008 2009 2010 2011 IRIN 2012 Eb dois 4 12 2 SH 100 fi 153 1 09 3 11 2 10 4 12 3 3 E C MgO 2 Median
21. ZORA E 20s v5 FA ISO IEC 13528 JIS Z 8405 PRAE Median NIQR 3 z 2006 2012 EE RSD C MgO RSDrob 2 1 2009 2012
22. 9 18 g ha 0 105 mg kg Table 16 9 1 7 mg 18 g ha pH 6 0 6 7
23. E 1992 SiO 9 S SiO gt 2 1
24. 57 Table 13 Change of the exchangeable Cd density of cultivated soil value of single AP 2 SP 3 4 test D i E difference regression analysis Year Season Test crops between the 2 3 mg kg mg kg AP SP processing 2009 Winter Spinach 0 036 0 002 0 037 0 002 ns 2010 Summer Spinach 0 038 0 002 0 036 0 003 n s 2010 Winter Qing geng cai 0 041 0 001 0 037 0 001 significance 2011 Summer Turnip 0 036 0 0004 0 035 0 003 n s 2011 Winter Spinach 0 039 0 001 0 035 0 002 significance 0 58 0 13 2012 Summer Carrot 0 037 0 001 0 032 0 001 significance 0 93 0 03 2012 Winter Spinach 0 038 0 001 0 032 0 003 significance 0 93 0 004 2013 Summer Carrot 0 038 0 001 0 031 0 001 significance 0 91 0 0005 9 1 Content of cadmium dissolved with pH 7 0 1 mol L ammonium acetate solution in the drying soil 2 Sludge fertilizer application plot 3 Standard plot 4 The p value which calculated from dispersion analysis for linear regression by examination start of each examination plot 5 Standard deviation n 4 2X2 repetition X number of samples 6 It is no significantly different for Processing examination section t test 5 of both sides leve
25. p 47 2013 18 p 106 1991 19 19 4 H p 4 1991 20 p 119 1991 21 BUR 22 49 58 1982 22 p 231 1989 23 25 83 100 1991 24
26. 3 T T R amp SE 2013 87 12 10 8 li 6 4 E SRS 8m 8m 941 5 E 4 ooQeoooQwooo dd T cd cd cd mb 60 60 c3 c c3 c3 c8 c8 A sY nf M Mag aso oa og pado d ap dE C eX STU Te ee D mg kg So Be 8 3 11 4 1 AE UM ad Ay E pL X X D2 at B jii ke BLV eim ICP AES 16 14 12 10 8 6 4 2 0 ee Ee 9 0 uoc 068 O9 09 toc 0 O9 0 Y T amp Gb 8 8 00 3 9 05 Co 0 08 66 6 amp 5 74 E ee pos EI e 96 e 4 2 ER 4 3 REEDED
27. 2 ER 139 1 JIS K8960 JIS K8731 JIS K9017 JIS K8121 sti Ye Zsh BLOX XH fe JIS K8905 JIS K8824
28. 5 101 107 2012 3 20 10 9 2008 4 HPLC 6 27 35 2013 5 Thompson M L R Ellison S Wood R The International Harmonized Protocol for the Proficiency Testing of Analytical Chemistry Laboratories Pure amp Appl Chem 78 1 145 196 2006 6 Horwitz W Protocol for the Design Conduct and Interpretation of Method Performance Studies Pure amp Appl Chem 67 2 331 343 1995 7 Thompson M Recent trends in inter laboratory precision at ppb and sub ppb concentrations in relation to fitness for purpose criteria in proficiency testing Analyst 125 385 386 2000 8 25 3 H 25 24 6116
29. E 96 Vol 7 2014 2 FAMIC 500 um
30. 9 IUPAC 2 1 2 3 2 3 kg TERS Retsch ZM1000 500 um 1 5 g 10
31. 9 45 38 20 1 8 4 6 30 1 DD
32. Ei ee criteria Criteria Approach LN v je XE 2 i 4 2 1
33. 1 m 5 50 mmX 230 mm 15 cm 35 2 mm EPL 65 24 Lik 500 um ZM200 Retsch 6 000 5 mL 2 mL ICP yet HGS3 pH EC 1 5 1 pH F 23 HORIBA EC F 54 HORIBA
34. 114 Vol 7 2014 y 0 0038x 0 61 p SS QR gl iy B J 3 C 4 C 23 0 700 os y 0 0033x 20 36 y 0 5912x 586 22 oan 650 Bt Ev ZR 21 0 z S im 600 20 0 m m E 190 Er 550 BL 18 0 500 5 C AMIR 1 200 y 2 6378x 975 a 1 100 bn B 1 000 fal iy 900 800 H 7 C 1C 115 a uu KE D 2013 mg kg 100 y 0 0014x 1 83 9 C 11 C y 0 0006x 0 47 10 C 125 y 0 1666x 80 5 D 100 bn ial 75 BL 50 0 5 10 15 20 12 C y 0 0065x 36
35. 11 75 45 2 64 4 6 2 4 6 2 a 7 120 mL 30 40 CA 4 4 1 b 30 His 53 30 C1 C 1 C MgO 1 4 6 2 AY C MgO E lt 15 30 45 60 75 C MgO 11 RAV TVG 11 12 E 4 6 2 a 4 4 1 c
36. 09 10 11 12 11 AVT 0 6 2 2 C MgO 4 v 10 0 08 4338 5 63 96 7 15 2 60 2 6 E 149 AEN FE 12 11 C MgO 0 7 6 0
37. 1 Cochran Grubbs 11 2 2 O 2 1 2 2 2 1 2 2 3 1 Table 3 1 Individual result of melamine mass Compound fertilizer Lab Calcium Calcium ae Compound Ammonium ID cyanamide 1 cyanamide 2 PORE gua fertilizer sulfate cyanamide A 274 281 0 384 0 380 0 828 0 837 0 202 0 208 0 0405 0 0383 B 2 827 2 36 0
38. 8 ISO 13528 2005 Statical methods for use in proficiency testing by interlaboratory comparisons JIS Z 8405 2008 9 AEEA 2012 6 61 83 2013 144 Vol 7 2014 Verification of Performance Characteristics of Testing Methods for Water soluble Molybdenum Content in Fertilizer by Sodium Thiocyante Absorptiometric Analysis Keiji YAGI Natuki TOYODOME Tokiya SUZUKP and Hideo SOETA Food and Agricultural Materials Inspection Center Fukuoka Regional Center Food and Agricultural Materials Inspection Center Fukuoka Regional Center Now Fertilizer and Feed Inspection Department We verified performance characteristics of testing methods for water soluble molybdenum W Mo by sodium thiocyanate absorptiometric analysis described in Testing Methods for Fertilizers The accuracy o
39. NH gt NH DS CI C l Y RN Y e C Fa N OH A A OH O O DO Clopyralid Aminopyralid Picloram CAS No 1702 17 6 CAS No 150114 71 9 CAS No 1918 02 1 Fig 1 Chemical structure of Clopyralid Aminopyralid and Picloram 2 1 40 C D x nt u 2 Vol 7 2014 500 um 2 1 99 DrEhrenstorfer GmbH
40. 1 A NO AS D 1 J 500 um 50 RER 2 10 1 1 5 E Ay Li ERAN HH 0 2 g 3 mol L 0 7 mL 0 2 mL 100 90
41. 39 1CP 4 2 61 S CaO S MgO 4 3 4 4 T S CaO 30 19 Median 30 09 NIQR 0 70 1 S MgO 4 59 Median 4 62 NIQR 140 16 5 pipe eS gs 3 5 EN 2H g LoO Co LO Qo LO CO LO QD lO C IO c IU OUS DT OUO OF TD Co re CO CO CO C COO CO C C CO wi XP XP DUE uu xu uu ux SL Ay VBR EP AI Yao DAS gt fas Big Bie 14
42. 7 NTOR NIOQR W Mo 0 210 GC NIQR 0 010 4 7 W Mo HorRat 0 92 AOAC 1 0 1 4 6 0 W Mo Te 7 NIQR RSDr PRSD HorRat
43. RSD ss RSDs HorRat Table 4 1 Table 4 4 HorRat HorRat RSDr PRSDR PRSDs Horwitz 0 0343 2 83 0 0015 0 04 0 8 4 5 96 0 0040 96 0 12 4 2 11 6 0 0346 1 60 0 0013 0 027 1 3 4 3 0 0024 0 06
44. 12 1 27 96 13 3 15 A 337 2001 2 p 112 120 2009 3 JIS K 8088 2010 4 JIS M 8217 1994 5 9 15 2011 6 FAMIC lt http www famic go jp ffis fert sub9 html gt bl Hr wad Y 1 gt 7 Thompson M R Ellison S Wood R The International Harmonized Protocol for the Proficiency Testing of Analytical Chemical Laboratories Pure amp Appl Chem 78 1 145 196 2006 8 JIS K 0131 X 1996 9 Horwitz W Protocol for the Design Conduct and Interpretation of Method Performance Studies P
45. 0 05 Table 8 10 0 1 mol L HCI Cd Eos 2 1 mol L HE pH 7 0 Cd 1 mol L HE pH 7 0 Cd Fig 4 2011 0 05 0 1 mol L HCI Cd 1 mol L HEZ pH 7 0 Cd Lk Table 12 13 pH v Table 1 5
46. X BR 1 FAMIC lt http www famic go jp ffis fert sub6 html gt 2 ISO IEC 17025 2005 General requirements for the competence of testing and calibration laboratories JIS Q 17025 2006 3 ISO Guide 34 2009 General requirements for the competence of reference material producers JIS Q 0034 2012 4 ISO Guide 35 2006 Reference materials General and statistical principles for certification JIS Q 0035 2008 5 ISO Guide 31 2000 Reference materials Contents of certificates and labels JIS Q 0031 2002 6 FAMIC lt http www famic go jp ffis fert sub9 html gt
47. 09 Dic nd 2011 2 1 SOLAAR S4 2 M 3 11 MK 41 1 8 T IA za 146 Vol 7 2014 1 g 1 mg 250 mL 4 z JUBRTR 20 mg mL 150 mL 30 C
48. 2 5 i HH E n ME 5 1 mol L HEZ pH 7 0 Cu 2013 i 7 pH 6 0 I 2 pH 6 0 pH 0258 ECO AVENE lt EDE 1 mol L 1 mol L MEZ pH 7 0 Zn 0 05 gt 0 05
49. 751 H E i HEZE pH 7 0 Cu VEZ pH 7 0 Zn FEDS 1 760 mg kg Table 2 EE 1 2 10a 6
50. 99 2 0 43 141 4 NET mw ee RED PHE coy W Mo 54 34 53 93 0 23 99 2 0 43 1 4 Mo 2 Mo 3 3 x100 4 2 2 3
51. Table 9 F 12 15 kg amp 10 33 kg 5 43 kg 4 58 kg gt 0 05 0 18 mg kg 0 15 mg kg 0 33 mg kg 0 28 mg kg THV lt 0 05 0 22 mg 0 17 mg 0 24 mg 0 18 mg CH 52 Vol 7 2014 0 05 0 05 0 34 mg 151 EE F
52. ne m 4 1 1 a T N vn 4 11 b A21a 4 3 1 a ee 45 la 4 11 1 a 4 4 10 1 a T Zn 4 9 1 a As 5 2 a Cd 5 3 a Hg 5 1 a Ni 5 4 a Cr 5 5 a n Pb 5 6 a 2A 3 1 1 A B C 3
53. 160 g 3 7 1 A rae E Al HO 3 1 a ef TN 4 1 1 a VLA EH 4 1 1 b ee T n ae s T C PzOs 4 2 3 a 20 mg mL H W K20 4 3 3 a C MgO 4 6 2 20 mg mL C MnO 472a 20 mg mL WOME I
54. Ms E rio Y LID HAASE 1A A 110 Vol 7 2014 3C C pa TEES T N T P20s T K20 T CaO O C 0 471 4 79 8 64 8 64 0 607 0 619 5 99 6 03 20 4 20 6 8 4 57 4 75 846 849 0 553 0 561 5 76 5 82 20 0 20 1 14 471 4 78 8 52 8 53 0 560 0 564 6 03 6 08 20 4 20 9 3C mg kg ate Pom T Cu T Zn As Cd 0 583 587 963 991 22 1 22 5 1 81 1 84 8 575 591 99 992 19 2 20 3 1 83 1 85 14 567 586 1 015 1 015 20 7 21 1 1 79 1 82 3C mg kg soe ene Hg Ni Cr Pb 0 0 464 0 470 73 3 74 3 78 6 81 2 36 4 36 5 8 0 448 0 478 74 2 74 6 80 5 80 5 35 1 35 1 14 0 443 0 473 78 3 78 7 75 4 79 4 36 1 36 9 15 5 11 5 y 0 0079x 14 878 2 y 2 0 0012x 10 72 St 15 0 St 11 0 R R ef jal 14 5 jal 10 5 14 0 10 0 0 10 20 30 40 2 A rr 111 2013 uu SI
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56. 49 d 20 1 y Jv 200 g Table 6 The design of the test plots lt Sludge fertilizer application plot AP gt Sludge fertilizer Ammonium sulfate Ammonium dihydrogenphosphate Potassium chloride Fused magnesium phosphate Total Standard plot SP Sludge fertilizer Ammonium sulfate Ammonium dihydrogenphosphate Potassium chloride Fused magnesium phosphate Total 1 Content as P205 2 Content as KO 4 The applied components Amont of application N p g g g 2000 66 104 323 68 115 200 40 134 144 321 68 170 20 104 127 200 40 88 144 2013 6 24 SERRE CURSSC 15 cm E CH EBLE 9 20 cm 7 17 8 1 8 16
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58. bu 0 09 C MgO 1 6 JIS K 8283 20 g 1 000 mL C MgO 11 12 11 1 9 w v96 2 0 ww 2 1 w y 2 C MgO 7
59. BE HPLC HPLC cm 2 1 Lv SIRE 500 um
60. BOR 1 1992 1992 2 FAMIC lt http www famic go jp ffis fert sub9 html gt 3 6 9 19 2013 4 Thompson M L R Ellison S Wood R The International Harmonized Protocol for the Proficiency Testing of Analytical Chemistry Laboratories Pure amp Appl Chem 78 1 145 196 2006 5 Horwitz W Protocol for the Design Conduct and Interpretation of Method Performance Studies Pure amp Appl Chem 67 2 331 343 1995 6 AOAC OFFICIAL METHODS OF ANALYSIS Appendix D Guidelines for Collaborative Study Procedures To Validate Characterist
61. Zn Sludge fertilizer application plot AP Zn Standard plot SP r2 o Cu Sludge fertilizer application plot AP Cu Standard plot SP uy Ui o e in Exchangeable Cu and Zn mg kg 0 0 Spinach Spinach Qing geng cai Turnip After winter cultivation 2010 After summer cultivation 2011 After summer cultivation 2010 After winter cultivation 2009 Spinach After winter cultivation 2011 Carrot After summer cultivation 2012 Spinach After winter cultivation 2012 Fig 5 Changes of the exchangeable Cu and Zn density of cultivated soil The error bar indicating the standard deviation Carrot After summer cultivation 2013 59 Table 14 Change of the exchangeable Cu and Zn density of cultivated soil Cu Zn Year Season Test crops APT SP AP sp mg kg mg kg mg kg mg kg 2009 Winter Spinach 0 40 0 07 0 40 0 03 13 0 1 1 2 0 2 2010 Summer Spinach 0 37 0 02 0 36 0 04 1 3 0 04 1 2 0 2 2010 Winter Qing geng cai 0 35 0 004 0 33 0 004 1 3 0 1 1 1 0 1 2011 Summer Turnip 0 29 0 002 0 28 0 01 1 5 0 1 1 3 0 3 2011 Winter Spinach 0 46 0 01 0 39 0 02 1 6 0 2 1 3 0 3 2012 Summer
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63. Horwitz 2007 2012 FED C MgO Median NIQR RSDyob HorRat 2011 C MgO E 1 2008 2010 ERU 2012 C MgO RSD 2 1 2 8 RSDrop 2 8 96 2007 4 E 2009 2011 A RSD 6 6 8 7 147 C MgO RSD 50 45 40
64. 70 Vol 7 2014 1 Mois 3 1 1 C 1 2 A N 4 1 2 1 C 1 D E HR 3 lt C PzOs 4 2 1 C d 4 2 3 E c 4 W P Os 4 2 1 C b 4 2 3 E E a 5 W K2O 4 3 1 C b 2 4 3 3 E 6 lt C MgO 4 2 1 C d 4 6 1 EDTA D b 4 6 2 E
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66. 5 ICP 3 10 10 22 mg kg Median 10 31 mg kg 90 NIQR 0 99 mg kg HSD 1 16 mg kg 4 2 A ICP H 5 86 Vol 7 2014 35 12 RS YE S2Ru8593529t 353m5 LL 99 OQ c uS 00 tL O 0 0 O0 Q1 1 am nac sm E NRI LEAN D OO Oe OD SS 3 A 2222 Ci Ce c 2002 a z mg kg U oA IE E 543 10 13 9 ii t TRUM
67. 3 3 20 64 Median 20 60 84 NIQR 0 20 HSD 0 45 11 14 lt 30 120 2013 83 4 W PzOs 134 133 1 3 4 12 05 Median 12 09
68. 0 0 0 1 mol L HCI Cd Table 12 0 1 mol L HCI Cd 2 2012 0 1 mol L HCI Cd E S 60 Vol 7 2014 0 0 23 p gt 0 05
69. 3 8 HPLC 13 Table 2 2 Homogeneity test results of ammeline No of 2 4 5 6 7 8 Sample 5 eae Sr RSD Sbb B ien RSDb r F Value sample 96 90 96 96 96 Calcium cyanamide 1 10 0 1 52 0 01 0 6 0 00 0 01 0 6 1 03 Calcium cyanamide 2 10 0 0 104 0 001 1 2 0 001 0 002 1 5 1 82 2 7 0 07 0 025 3 6 2 57 Calcium cyanamide Compound fertilizer 10 0 0 194 0 002 0 9 0 000 0 002 0 9 1 01 Ammonium sulfate 10 0 0 0367 0 0011 3 1 0 0 0011 3 1 0 47 1 10 Refer to the footnote of Table 2 1 Table 2 3 Homogeneity test results of ammelide No of 2 A E 6 5 Sample m 5 J RSD Sbb E S b RSD F Value sample 96 90 96 96 90 Calcium cyanamide 1 10 0 1 12 0 02 1 8 0 02 0 03 2 3 2 37 Calcium cyanamide 2 10 0 0 367 0 011 3 1 0 0 011 3 1 0 56 Compound EEC io s FT CU 3 3 0 005 0 007 4 1 2 16 Calcium cyanamide Compound fertilizer 10 0 0 724 0 025 3 5 0 012 0 028 3 9 1 48 Ammonium sulfate 10 0 0 0354 0 0038 10 7 0 0017 0 0042 11 7 1 52 1 10 Refer to the footnote of Table 2 1 Table 2 4 Homogeneity test results of cyanuric acid No of 2 4 5 6 7 8 Sample ur Sr j RSD Sbb A RSDb r F Value sample
70. 2 Tit oo E D OR 1E f ZE 0 ow sw c vec a anb on uil TS E wt 20 b pt 30 c 2013 109 n sg Sw u 3A A pali T N A N C P20s W K20 0 14 83 14 95 10 59 10 62 10 09 10 14 13 18 13 56 12 14 80 14 80 10 78 10 90 10 11 10 14 13 68 13 72 20 14 77 14 91 10 89 10 91 9 88 10 23 13 70 13 74 24 14 50 14 53 10 60 10 75 9 96 10 04 13 48 13 83 28 14 62 14 63 10 71 10 74 10 01 10 06 13 64 13 75 32 14 55 14 56 10 72 10 75 10 07 10 07 13 45 13 56 38 14 69 14 70 10 70 10 73 9 99 10 04 13 36 13 48 3A ua EEEE qe SES C MgO C MnO C B205 0 3 200 3 44 0 389 0 414 0 204 0 210 12 3 20 3 35 0
71. H ts 107 i I nu 2013 2A A sek ST TTS ME TIENS YL AS ig zi BH Jo ALY T N 4 1 1 a PUN ETE 4 1 1 b nne x em E z F S vy H v y A N 4 1 2 b 1 20 Ye C P 4 2 3 2 L C PzO5 3 a 20 mg mL PRIME LH W KeO 4 3 3 a api E C MgO 4 6 2 a 20 mg mL C MnO 472a lt 20 mg mL nly de TT RF BE E PA C C B203 4 8 1 a 20 mg mL 1 2B
72. SRM Table 1 Operating conditions of LC MS MS Column Waters ACQUITY UPLC HSS C18 2 1 mm id x100 mm L 1 8 um particle size 5 A Formic acid 1 1 000 B Methanol Mobile phase gt 0 min 5 B 5 min 60 B 6 min 95 B 7 min 5 B Flow rate 0 4 mL min Column temperature 40 C Tonaization Electrospray ionization ESI Mode Positive Desolvation gas N2 400 C 800 L h Cone gas Ar 50 L h Capillary voltage 1 0kV Ion source 120 C Table 2 MS MS Parameters Product ion Collision energy Agricultural Precursor for for Cone for for chemical ion quantification identification voltage quantification identification m z m z mz V eV eV Clopyralid 192 146 110 20 20 30 Aminopyralid 207 161 189 22 22 16 Picloram 241 195 223 28 22 16 5 SRM Scheme 1 4 Vol 7 2014 ce Sample 5 00 g Erlenmeyer flask with stopper 200 mL Sodium hydroxide 40 g L
73. 0 4 0 4 E 20 Vol 7 2014 X 1 23 4 H 15 A 23 524 2011 2
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76. 0 1 mol L HCI Cd LAL Codex 14 mg 36 gha 5 X ER vAO HERR xo B 1
77. E 2012 4 2009 4 2012 4 GA Et E 1 EE gt I Lu 151 E 2013 JENI 7 EKET v I YO AG BOA Lu Ea I Y
78. 1 ww 0 1 1 EE 0 1 mol L HCI Cd E 5 32 0 1mol L 1 5 mg 90 3 0 05 yet HZ m2 63 Table 16 Change of the 2009 2013 year of the quantity of cadmium load by fertilizer quantity of peculating due to Year 2009 2009 2010 2010 2011 2011 2012 2012 2013 0 1 mol L HCLCd mg kg Quantity of cadm
79. 0 66 0 13 98 4 101 0 S SiO S SiO gt AOAC 10 100 95 102 TE H 5 S SiO gt wew PIMEC MERE ie AD 9 9 p c 95 9 p p p c 96 S SiO2 40 40 39 34 0 66 1 6 98 4 0 1 0 3 S SiO2 25 25 25 13 0 13 0 5 100 5 0 2 0 9 S Si02 10 10 10 10 0 10 1 0 101 0 0 04 0 4 1 9 SiOz DAA E GHE 2 3 3 4 C B A 5 D C A x100 6 E B A X100 7 3 8 G F B x100
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81. Cochran Grubbs 10 c f 1 a d e 2 Table 2 Collaborative study results Mass fraction Lab ID Solid sample a Solid sample b Solid sample c A 8 17 8 25 12 54 12 53 245 1 246 4 B 9 07 9 13 13 24 13 52 253 0 252 7 C 9 13 9 20 13 29 13 20 254 5 253 7 D 8 31 8 22 12 38 12 48 246 1 241 4 E 8 05 8 21 12 27 12 20 247 8 246 4 F 8 32 8 35 12 51 12 62 247 0 246 0 G 8 40 8 40 12 57 12 55 244 5 243 8 H 8 35 8 48 12 56 12 59 246 4 245 8 I 8 35 8 41 12 70 12 68 245 8 245 8 J 8 42 8 43 12 78 12 89 246 5 246 2 Lab ID Solid sample d Liquid sample e Liquid sample f A 246 1 245 8 1 40 1 39 2 87 2 86 B 252 1 253 0 1 46 1 49 2 92 2 91 C 254 5 254 0 1 50 1 50 2 94 2 94 D 245 7 245 2 1 40 1 40 2 86 2 86 E 246 7 245 9 1 41 1 41 2 88 2 88 F 246 7 245 4 1 40 1 41 2 88 2 88 G 244 0 244 2 1 41 1 41 2 88 2 88 H 245 5 246 1 1 42 1 41 2 89 2 89 I 245 6 245 9 1 41 1 42 2 88 2 88 J 245 9 245 6 1 42 1 41 2 89 2 93 1 Outlier By Cochran 2 Outlier By Grubbs 3
82. 2 RE e f a b e f 7 g WERE H RL c d 1 5 g 2 12 2 3 MZ MZ I a b 3g
83. EAMIC A 1 E LL ee 3 oi ts AKES HAAR ip fe 10 22 28 36 43 68 95 9 2013 FAMIC A 10 FAMIC B 10 FAMIC C 12 m 105 lt gt 10 os aces ace Sls e s we EE EE e sie eva e EE EE ECE EE ER eid 123 11 OECD
84. 8 gt 2013 69 Lk 9 19 9 1 4 4 7 1 9 1 200g THY 220 Ee 4 alli HNL 212 um
85. X BR 1 ISO IEC 17025 2005 General requirements for the competence of testing and calibration laboratories JIS Q 17025 2006 2 Codex Alimentarius Commission PROCEDURAL MANUAL Twentieth edition 2011 lt ftp ftp fao org codex Publications ProcManuals Manual_20e pdf gt 3 FAMIC lt http www famic go jp ffis fert sub9 html gt 4 1992 1992 5 59 3 16 700 26 9 1 1148 2014 6 AOAC Guidelines for Single Laboratory Validation of Chemical Methods for Dietary Supplements and Botanicals AOAC INTERNATIONAL 2002 7 Codex Guideline on Analytical Terminology CAC GL 72 2009 2009
86. 90 NIQR 0 38 HSD 0 33 4 5 20 0 ee 20 1 0 9 ER d 5 O O OY 0o 00 m m CI ON N CI CI CA NN CX CX 22 2 2 2 2 2 2 2 3 3 Dt 5 W K20 132 65 57 HIE 4 3 5 11 70 96 Median 11 74 89 NIQR 0 35 HSD 0 32 21 2 RES Xa 11 8 12 0 12 2 12 4 12 6 12 8 13 0 13
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88. 09 11 10 12 20 2 600 60 cm
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90. 2013 EAMIC A 13 101 4 ISO Guide 31 2000 JIS Q 0031 2002 6 ISO Guide 33 2000 JIS Q 0033 2002 1 u ISO TS 21748 2004 JIS Z 8404 1 2006 sw ss RRES p 8 10 6 a z b 2
91. lt C MgO 2 Lu 3 2013 143 82 1 3 Mois A N amp TRTIEO Z0 R8 C P205 W P205 W K20 C MgO W MgO lt C MnO lt C B203 TAs TCd 11 Lie 2 cm Lu S SiO gt AL C MsgO 3 1992
92. 7 Thompson M R Ellison S Wood R The International Harmonized Protocol for the Proficiency Testing of Analytical Chemical Laboratories Pure amp Appl Chem 78 1 145 196 2006 8 ISO 5725 2 1994 Accuracy trueness and precision of measurement methods and results Part 2 Basic method for the determination of repeatability and reproducibility of standard measurement method JIS Z 8402 2 1999 2 i 9 AOAC OFFICIAL METHODS OF ANALYSIS Appendix D Guideline for Collaborative Study Procedures To Validate Characteristics of a Method of Analysis AOAC INTERNATIONAL Gaithersburg 2005 10 Thompson M Recent trends in inter laboratory precision at ppb and sub ppb concentrations in relation to H fitness for purpose criteria in proficiency testing Analyst 125 385 386 2000 11 Codex Alimentarius CODEX ALIMENTARIUS COMMISSION PROCEDURAL MANUAL Twentieth edition p66 2011 12 ISO Guide 33 2000 Uses of certified reference materials JIS Q 0033 2002 13 ISO TS 21748 2004 Measurement uncertainty Part 1 Guidance for the use of repeatability
93. criteria Criteria Approach B pr IS E 1992 W Fe
94. Te 7 Het NIQR RSDr PRSD HorRat MARD ROHR cere ee AO 2 Pa DI P W Fe 2012 86 0 240 0 013 5 4 5 0 1 09 1 PRE 2 3 NIQR 4 C B A x100 5 Horwitz 6 HorRat E C D 4 W Fe 1 k Fe ELTE FER 0 05 10 SSATAMRRE ZO COJZKYAT E W Fe 136 Vol 7 2014 101 1 107 0 1 1 7 0 2 W Fe 0 01 967 1 W Fe MAIL 103 6 105 7 3 6 5 7 3 W Fe 0 01
95. lt http www famic go jp ffis fert sub6 html gt 2 ISO IEC 17025 2005 General requirements for the competence of testing and calibration laboratories JIS Q 17025 2006 3 2010 FAMIC A 10 FAMIC B 10 4 107 121 2009 4 2012 FAMIC C 12 6 84 100 2013 5 ISO Guide 34 2009 General requirements for the competence of reference material producers JIS Q 0034 2012 6 ISO Guide 35 2006 Reference materials General and statistical principles for certification JIS Q 0035 2008 7 ISO Guide 31 2000 Reference materials Contents of certificates a
96. pH 0 1 mol L HCI Cd 2009 2010 0 05 2 Table 11 es gt 0 05 2010 ON ree ee lt 0 05S gt 0 05 2 Table 11 2011
97. seee 131 12 P 2 138 13 Tt js 145 Research Report of Fertilizer Volume 7 2014 Index lt Development and Validation for Determination Methods gt 1 Determination of Clopyralid Aminopyralid and Picloram in Compost and Composted Sludge Fertilizer by Liquid Chromatography Tandem Mass Spectrometry LC MS MS Hisanori ARAYA Toshiharu YAGI Yoshimi HASHIMOTO and Yuji SHIRAI 1 2 Determination of Melamine and Its Related Substances in Fertilizer by High Performance Liquid Chromatography HPLC A Collaborative Study n Etsuko BANDO and Sigehiro KAI ecco 10 3 Determination of Organic Carbon in Sludge Fertilizer and Compost by Hydrochloric Acid Treated Combustion Method A Collaborative Study n Aiko YANO and Yuji SHIRAI ecco n 22 4 Testing Method of the Total Amount of Sulfur Content as Sulfur Trioxide A Collaborative Study n Shin ABE Chika SUZUKI and Yuji SHIRAI ecco 28 5 Determination of Soluble Silicic Acid in Fertilizers Containing Silica Gel Fertilizer by Potassium Fluoride Method A Colla
98. 1 06 1 43 1 12 1 59 1 48 1 57 1 58 1 31 1 68 1 26 1 06 1 46 1 28 1 09 1 59 1 69 1 63 1 34 1 65 1 36 HH 1 06 1 44 1 45 1 07 1 61 1 55 1 78 1 35 1 62 1 35 1 12 1 43 1 33 1 15 1 48 1 53 1 79 1 29 1 67 1 31 amp 3 3 15 02 14 85 15 11 14 95 14 81 14 84 14 86 14 73 14 66 14 86 14 90 14 89 14 99 15 10 14 76 15 19 14 9 14 82 14 58 14 86 LENS 14 9 14 89 14 81 14 89 15 00 14 99 14 80 14 53 14 77 14 83 14 77 14 36 14 88 14 80 14 76 14 76 14 61 14 56 15 00 14 79 14 99 14 79 14 97 14 94 14 84 14 80 14 85 14 75 14 46 14 94 14 82 14 98 14 92 14 78 14 80 15 18 14 77 14 71 14 58 14 98 2013 FAMIC A 13 99 3 A 10 66 10 57 10 58 10 61 10 55 10 57 10 72 10 73 10 77 10 71 10 69 10 90 B 10 65 10 73 10 56 10 49 10 65 10 51 10 83 10 78 10 69 10 82 10 71 10 63 C 10 28 10 33 10 32 10 06 10 14 10 14 10 7
99. 5 0 8 g 50 2 10 qd 2 Ue 3 0 50 g 200 mL 1 15 100 mL ib Tn n H 4 fag HPLC 11 30 50 mL
100. PARE c d 1 g 0 1 mg 200 mL 50 mL RRR CHEV 5 250 mL 3 e f e f 5 g 5 mL 50 mL a b pH I 100 mL DHA mL 2 1 1 mL Uv Ai 100 g L 9 6 C 80 90 4 0 1 mg 80 90 1 OME d 2 1
101. uu 40 20 11 1 11 3 11 5 11 7 11 9 12 1 12 3 12 5 12 7 2x ei Sx 0 3 5 3 6 Ex ee See wktbLu 7 W MgO 120 109 7 ICP 4 EDTA 3 7 3 75 Median 3 79 99 NIQR 0 68 HSD 0 12 ICP 5
102. 1 1 45 mL 5 mL MERRER M 2 mL 16 mL TI 10 mL 460 nm 1 3 W Mo 4 14 1 a 4 1 3 1 3 4
103. 8 ISO 13528 2005 Statical methods for use in proficiency testing by interlaboratory comparisons JIS Z 8405 2008 9 AEEA 2012 6 61 83 2013 137 Verification of Performance Characteristics of Testing Method for Iron in Fertilizer by Atomic Absorption Spectrometry Shinei TAKAHASHI Chika SUZUKI and Noriyuki SASAKI Food and Agricultural Materials Inspection Center Sendai Regional Center Now Fertilizer and Feed Inspection Department Food and Agricultural Materials Inspection Center Sendai Regional Center We verified performance characteristics of testing method for water soluble iron W Fe by atomic absorption spectrometry described in Testing Methods for Fertilizers The accuracy of testing methods for the several form of iron was assured from 3 replicate determinations of 6 fertilizer samples containing 0 01 96 10 96 iron which were prepared each test As
104. A N 136 130 5 1 3 2 9 87 Median 9 92 VOREL NIQR 0 74 HSD 0 28 25 20 15 10 5 0 ie co cuca 16 qc ee 8 ELIO A iL Oo 9 x 90 9 oo TO et ue es cdd si ed CS om E Lom O Slll Pos AD 8B E 7 o S 3 1 3 2 apu uii 3 C PzOs 129 128 1 ICP
105. HB ME 2007 1 152 167 2008 5 ot 2008 2 97 115 2009 6 HB JE EISE JOKE Fia 2009 3 73 94 2010 7 lj Nas zl T L iI ze 7
106. 212 um PRSDs HHL PRSDs X0 5 PRSDk X2 C MgO RSD PRSDs PRSDRX2 Codex RSDk PRSDk X2 HorRat 2 C MgO PRSDs X2 PRSDs X2 RSD Horwitz C MgO RSDrov
107. a lt C MgO 0 0 31 0 20 25 30 CC 5 C MgO 11 lt 11 A 12 20 C 11 C MgO C MgO 12 C MgO 30 C 2 63 20 C CHE 30 C 2 96 20 C 30 C 11
108. z gt I3 119 8 94 25 95 P205 24 P P205 4 4 P 9 38 400 nm 410 nm 415 nm 420 nm
109. 127 3 7 S SiO 6 B x10 x2xt n 1 0 05 S SiO 2 0 3 0 1 S SiO S SiO 10
110. 77 5 1 Pu Eod Median NIOR RSDop HorRatrop HSD n R mgkg 96 mglkg mg kg C MgO 2007 137 3 41 0 07 22 0 65 0 11 2008 142 4 62 0 12 2 5 0 80 0 15 2010 137 3 11 0 07 2 4 071 0 10 2011 128 2 48 0 07 2 8 0 81 0 09 2013 129 6 18 0 13 2 2 071 0 19 W MgO 2011 119 1 94 0 09 4 6 1 28 0 07 2012 116 1 68 0 05 3 1 0 83 0 06 2013 120 3 79 0 68 18 0 5 50 0 12 C MnO 2009 126 0 54 0 02 3 6 0 83 0 02 2013 Vi AACN ER BR SE 6 eoe 115 0 51 0 01 2 8 0 64 0 02 W MnO 2012 112 1 25 0 03 24 0 61 0 05 C B203 2009 Mis pc b ESE s pel 120 0 28 0 02 5 6 1 16 0 01 2013 5 ARC BES SE 104 0 25 0 01 5 5 1 11 0 01 W B203 2006 132 0 40 0 02 42 0 91 0 02 2008 119 0 26 0 01 2 9 0 58 0 01 2010 116 0 29 0 01 3 4 0 70 0 01 2012 103 0 240 0 009 3 6 0 72 0 012 Fe 2012 86 0 240 0 013 54 1 09 0 012 Cu 2012 88 0 0545 0 0014 2 6 0 42 0 0034 Zn 2012 87 0 0595 0 0029 4 8 0 78 0 0036 Mo 2012 52 0 210 0 010 47 0 92 0 011 T As 2006 84 1 89 0 19 10 1 0 70 0 27 2007 68 3 84 0 38 9 8 0 75 0 50 2008 65 4 14 0 41 9 8 0 76 0 53 2009 59 4 31 0 60 13 9 1 09 0
111. 5 EH 5 0 17 mg kg 7 mg 14 mg mol L HCI Cd DEN EU 0 1 mol L HCI Cd NM 1 5 mg 12 g ha 2009 4 0 05 RLT m 400 kg 3 42 mg gt 0 05 Table 15 47 mg
112. Mo 0 002 0 0006 0 0003 AOAC 0 001 80 115 Mo 0 002 W Mo 0 003 0 01 6 She gt ENS 1 Wes 2 es yd o A Wa ERE T W Mo Mo 0 02 0 02 0 0202 0 0006 0 006 0 003 W Mo Mo 0 002 0 002 0 00171 0 00006 0 0006 0 0003 1 Mo 2 7 3 x10 4 x2xt n 1 0 05 4
113. 9 1 9 1 HL 4 7 17 9 RL 1 180g 165 SA I 1 1 2 3 4 5 6 7 2 1 3 2 3 1 5 3 6 7 4 4 2 i EAS 7 7 8 6 5 4 8 9 8 9 7 9 8 2 IUPAC ISO AOAC 2 1 10 BR IN C Pz0s C MnO
114. ae W xVz V1 x34 3 x Ws g Ws V Vo m mL mL 4 IUPAC ISO AOAC 10 2 9 X K DAE g Wx WB x0 3430 W x V V 1 x100 CHEVY 30 Vol 7 2014 1 g 5 8 Weigh to the order of 0 1 mg into a 200 mL tall beaker Analytical sample lt About 50 mL of potassium hydroxide etanol solution Cover with a watch glass and boil Standing to cool Transfer 250 mL volumetric flask water Water up to the marked line Filtration Type 3 filter paper Aliquot predetermined amount a RS lt About 50 mL water lt About 5 mL hydrogen peroxide Heating 80 C 90 C 1 hour Standing to cool lt A few drops of phenolphthalein solution 1g 100 mL Hydrochloric acid 2 1 until the solution beco
115. 2012 gt 0 05 2013 0 05 2009 0 1 mol L HCl Cd 15 B 2011 0 05 0 1 mol L HCl Cd 1 mol L MEZ PH 7 0 Cd lt 0 05 TT gt 0 05 LAL 1 5 mg
116. BE oa ao s ee ah zi X R 1 ISO IEC 17025 2005 General requirements for the competence of testing and calibration laboratories JIS Q 17025 2005 2 FAMIC lt http www famic go jp ffis fert sub6 html gt 3 ISO IEC 17043 2010 Conformity assessment General requirements for proficiency testing JIS Q 17043 2011 4 Thompson M
117. RSDu 1 1 5 2 M Table 2 Homogeneity test results No of Mean Ge RSD su Sor RSDpar 9 10 Sample 1 e 3 3 3 F value sample 90 96 90 90 96 Calcined sludge fertilizer 10 0 8 82 0 46 5 2 0 00 0 46 25 2 0 20 Industrial sludge fertilizer 10 0 15 10 0 52 3 4 0 00 0 52 3 4 0 65 Compost 9 1 21 46 0 92 4 3 0 00 0 92 4 3 0 58 Human waste sludge fertilizer 10 0 36 01 0 39 1 1 0 12 0 41 1 1 1 20 Composted sludge fertilizer 10 0 38 19 0 44 1 2 0 00 0 44 1 2 0 67 1 The number of samples used for analysis The number of outliers 2 Grand mean value n The number of samples used for analysis X The number of repetition 2 3 Mass fraction 4 Standard deviation of repeatability 5 Relative standard deviation of repeatability 6 Standard deviation of sample to sample 7 Standard devitation of sample to sample including repeatability Spip al Sup s 8 Relative standard deviation of sample
118. sp RSDr HorRat HorRat HorRat Horwitz T zu Table 3 Statistical analysis of collaborative study results No of labs Mean Re RSD sa Sample 1 E 4s i 3 P 96 96 96 96 Phosphate fertilizer mixture 1 8 24 99 0 16 0 6 0 33 Phosphate fertilizer mixture 2 8 34 50 0 26 0 7 0 48 Compound fertilizer 1 8 30 30 0 13 0 4 0 60 Compound fertilizer 2 8 33 34 0 13 0 4 0 47 Compound fertilizer 3 8 15 76 0 11 0 7 0 21 1 Number of laboratories where p 2number of laboratories 2 Grand mean value n The number of participating testing laboratories p X The number of repetition 2 3 Mass fraction 4 Standard deviation of repeatability 5 Relative standard deviation of repeatability 6 Standard deviation of reproducibility 7 Relative standard deviation of reproducibility 8 Horwitz ratio of reproducibility 4 RSDr iX RSD RSD P PRSDg
119. 2 z 2 lt Il 3 3 z d Median NIQR RSD HorRat E 7 NIQR RSDr p HorRatrop HSD 6 1 ll 2 135 136 108 120 117 111 119 89 93 47 53 53 69 53 53 67 E 99 100 84 90 89 86 99 77 89 90 82 88 88 87 87 85 Median 1 Horwitz Median f 2 z 3 Sigh 1 1 0 0 0 0 7 5 14 11 9 7 4 8 6 5 6 5 12 9 1 1 0 0 14 12 12 10 4 4 7 7 3 2 4 3 5 9 14 4 3 5 6 3 4 7 11 1 2 3 5 5 8 2 3 10 13 3 z 3 Izl 74 Vol 7 2014
120. 95 2 o a 0 kxu ho b j sp Sw n 6 k kx 2 2
121. 0 1 mol L HCI Cd 33 2012 lt 0 05 2011 2009 2012 gt 0 05 2013 0 0 2013 FE His o 1 mol L pH 7 0 Cd 2011
122. 17 ob AF EST MAE fin j HE T 2006 1 138 2007 4 EIR 1 1 2011 18 BAEZ XE 19 AEEA HE HH JON aspire E
123. 7 W MgO 4 6 1 C b 4 6 2 Eick 0 8 C MnO 4 2 1 C d 4 7 3 E 9 C B203 4 2 1 C d 4 8 3 E 2 10 TAs 5 24 1 D a 1 E 5 24 2 E 11 TLCd 3 6 1 D a 1 R E a 5 19 1 E 12 S SiOz 4 4 1 B b 4 4 3 D 13 AL 4 5 1 1 C b 4 5 2 2
124. 2 2 37 1 g analytical sample Weigh to the order of 1 mg to a 300 mL tall beaker About 150 mL hydrochloric acid 1 23 about 30 C At 30 C 2 C for 1 hour while shaking to mix every 10 minutes Standing to cool Supernatant filtration Washing with water lt Filtrate gt Water up to the marked line Sample solution 1 lt About 150 mL sodium hydroxide 20 g L about 65 C Shaking to mix Room temperature Type 6 filter paper 250 mL volumetric flask Transfer residue to a filter paper lt Residue gt Together with filter paper 250 mL volumetric flask made of polymer Stopple and shake to mix until a filter paler breaks down 65 C 2 C 1 hour shaking to mix every 10 minutes Standing to cool Water up to the marked line Sample solution 2 Aliquot pred
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126. 5 2 2007 6 6 2009 8 7 96 2011 6 8 P RSD 3 6 au 5 128 119 7 420 nm 83 70 96 400 nm 410 nm 415 nm 31 26 1
127. Vol 7 2014 2 1 RSD 11 11 0 75 1 2 12 11 C MgO OW it A Lr 15 75 2 55 992 65 15 60 60 12 C MgO igs 3i C MgO C MgO 3 12 C MgO 15 7 27 75 7 29 Lr 60 2 98 3 4 75
128. 2 000xg 5 50 mL 4 1 1 5 mL 8 000xg THI LYE AUK HPLC Scheme 1 Table 1 gt Sample 0 50 g Erlenmeyer flask with stopper 200 mL lt Hydrochloric acid water 1 15 100 mL Extract by ultrasonic wave for 30 min 200 5 min zr Dilute aliquots extraction liquid with acetonitrile phosphate buffer 4 1 8 000 5 mm HPLC Scheme 1 Method flow sheet of melamine and related substances in fertilizer Table 1 HPLC conditions Column TOSOH corporation TSKgel Amide 80 4 6 mm i d x250 mm L 5 um parti
129. 50 30 1 90 Lu 30 CH UIE 85 8 2012 2012 30 30 240 E 2013 30 151 x I 118 54 Vol 7 2014 Z 30
130. C MgO 2013 C MgO 1 C MgO RSDrop 3 6 x R 1 ISO IEC 17025 2005 General requirements for the competence of testing and calibration laboratories JIS Q 17025 2005 2 ISO IEC 13528 2005 Statistical methods for use in proficiency testing by interlaboratory comparisons JIS Z 8405 2008 3 ot 2006 HE 1 138 151 2008 4
131. JISK8815 7 0 1 g 100 mL 95 100 mL 8 1 g 100 mL 95 100 mL 9 JISK JIS K 8896 0 10 g JIS K 8102 250 mL 750 mL TY f 0 1 g 100 mL 8799 1g JISK8102 125 4 S SiO 3 1 XO S SiO gt 4 4 1 a 4 1
132. W Mo 5 Te W Mo 0 W Mo 0 1 2 5 0 001 0 01 100 2 96 100 8 W Mo AOAC 1 92 967 105 96 0 1 90 108
133. 2 3 6 9 0 188 1 10 0 004 0 028 96 2 1 3 9 0 052 0 08 6 5 7 6 0 0345 0 0031 8 9 0 003 2 0 014 3 0 0056 0 3 amp 0 09 0 Hg ci Aimi TRNK I 06 IL 0 105 x f Hj d EA 3S d 0365 IZT 4 2 96 0 0067 B 3 amp n
134. C MgO 79 68 7 EDTA 4 ICP 4 5 3 88 Median 3 77 ATRE 85 NIQR 0 14 HSD 0 12 13 10 5 EDTA 1523 4 ICP 1 EDTA 5 2013 89 C MgO RSD
135. T F A AGRIS JIS K8107 EDTA Na 2 uu ERES Mo 2 5 Mo 0 1 Mo 0 02 Mo 0 002 20 10 10 5 10 10 14 10 10 3 10 4 64 0 185 0 037 0 0037 51 36 59 815 49 963 10 10 10 1 9963 90 Mo 2 5 0 1 0 02 0 002 3 1 Elix Advantage 5 JIS K 0557 A3 2 JIS K 8951 3 JIS K 8223 4 WER M R JIS K 8981 S g 1 1 10 mL L 100 mL 5 JIS mL 6 T JISK8136 500 mL 1c 7
136. Vol 7 2014 ES 4 0 95 96 45 15 0 24 0 5 1 S SiO gt 6 2 2 zm 3 S SiO 5 E S SiO gt 10 40 VC RETE S SiO
137. 1 gr il il il E co RF Rt ke kK il 50 1 2 a 4 Ba 4 Ba NEA 3 10 Waters 2695 Series LC 10A Series Agilent technologies 1100 Series fi Waters 2487 Agilent technologies 1100 Series Waters 2695 Seri
138. 0 89 2011 0 0 2011 0 1 mol L HCI Cd gt 0 25 ro 020 l T i T T I T 9 l 1 _ i J 0 15 z E x 3 oio Sludge fertilizer application plot AP Standard plot SP Carrot Spinach Spinach Qing geng cai Turnip Spinach Carrot Spinach Carrot 2009 2010 2010 2011 2011 2012 2012 2013 Fig 3 Changes of the 0 1 mol L HCI Cd density of cul
139. 4 Je 5 mg kg 2 ERU 18 4 m 100 mg EL I I Lu 2 2 5 2 6 EE E Kr E dfi ILE E 0 1 mol L
140. IER 3 2 Jj lt E aX 88 75 35 2388 HE cm X E x re 2013 121 nul FEE ol X 1 FAMIC
141. W Fe men TREC ose mR BERE amao AD 95 p 95 c 95 p pe 96 p p GA W Fe Fe 10 10 10 11 0 11 1 1 101 1 0 06 0 6 Fe 0 5 0 5 0 5138 0 01 2 8 102 8 0 001 0 2 Fe 0 05 0 05 0 0535 0 0035 7 0 107 0 0 0018 3 3 Fe 1 1 1 036 0 036 3 6 103 6 0 002 0 2 Fe 0 1 0 1 0 1057 0 0057 5 7 105 7 0 001 0 6 Fe 0 01 0 01 0 01051 0 00051 5 1 105 1 0 000052 0 5 D W Fe 2 3 3 4 C B A 5 D C A x100 6 E B A X100 7 3 8 G E B x100 3 2 AOAC 7 x10 H H FERS RY eli HII E OO TCR 45 BF E W Fe 6 28 x2xt n 1 0 05 JOT H Ed 0 01 85 967 110 0 001 80 967 115 W Fe Fe 0 01 KUW ME
142. 0 46 mg Table 9 Cadmium uptake and yield of carrot in the test Part Unit Test plot 1 Test plot 2 average t test lt Sludge fertilizer application plot AP gt 11 50 5 20 16 70 1 23 0 71 1 94 Fresh weight Dry weight Root Leaf Total Root Leaf Total Root kg kg kg kg kg kg mg kg 0 17 0 20 12 80 5 65 18 45 1 26 0 72 1 98 0 16 0 19 12 15 5 43 17 58 1 25 0 71 1 96 0 18 n s Ld Cadmium concentration Quantity of cadmium uptake Leaf Root Leaf Total mg kg mg plot mg plot mg plot 0 34 0 21 0 24 0 46 0 35 0 25 0 25 0 50 0 32 0 20 0 23 0 43 0 32 0 23 0 23 0 46 0 33 0 22 0 24 0 46 PAETA 4 significance significance significance significance lt Standard plot SP gt 11 30 5 00 16 30 1 21 0 71 1 91 Fresh weight Root Leaf Total Root Leaf Total Root kg kg kg kg kg kg mg kg 9 35 4 15 13 50 Dry weight 1 00 0 56 1 56 0 16 0 17 0 14 0 14 10 33 4 58 14 90 1 10 0 63 1 74 0 15 r x Cadmium concentration Quantity of cadmium uptake 1 Content in the drying soil Leaf Root Leaf Total mg kg mg plot mg plot mg plot 0 31 0 16 0 17 0 34 0 30 0 17 0 17 0 34 0 26 0 17 0 19 0 36 0 26 0 16 0 18 0 34 0 28 0
143. E I Lu 66 Vol 7 2014 471 210 2162009 30 ARMY 31 E51 EO i ES WU A 32 lt http www niaes affre go jp techdoc cadmium_control pdf gt H 124 127 TEACH E 1991 J 34 127 74 81 2010 49 2011 67 Effect of Continuous Application of Sludge Fertilizer on Cadmium Absorption of the Crop and Accumulation of Cadmium in the Soil Continued Report Toshiaki HIROI Souichi IGARASHI Masahiro ECHI Yoshimi HASHIMOTO and Fumihiro ABE Food and Agricultural Materials Inspection Center Fertilizer and Feed Inspection Department Food and Agricultural Materials Inspection Center Fertilizer and Feed Inspection Department Now Fukuoka Regional Center Food and Agricultural Materials Inspection Center Fertilizer and Feed Inspection Department
144. 33 fag SO 100 HEE IUPAC AOAC S 2 4969 RSD ss RSDr HorRat HorRat Table 3 HorRat HorRat RSD PRSD PRSDg Horwitz S 0 564 99 17 sg 0 001 0 24 0 003 1 39 ATHV RSD XU RSDr 0
145. ie oU FH X 1 ISO IEC 17025 2005 General requirements for the competence of testing and calibration laboratories JIS Q 17025 2006 2 Codex Alimentarius Commission PROCEDURAL MANUAL Twentieth edition 2011 lt ftp ftp fao org codex Publications ProcManuals Manual_20e pdf gt 3 FAMIO lt http www famic go jp ffis fert sub9 html gt 4 1992 1992 5 59 3 16 700 26 9 1 1148 2014 6 AOAC Guidelines for Single Laboratory Validation of Chemical Methods for Dietary Supplements and Botanicals AOAC INTERNATIONAL 2002 7 Codex Guideline on Analytical Terminology CAC GL 72 2009 2009 lt www codexalimentarius net download standards 11357 cxg_072e pdf gt
146. k 2 d 7 n 2 Uc am 4 2 120 Vol 7 2014 HS Ymeas U meas 4 UcrM Am Uc Am A T N 9 14 70 0 05 14 71 0 04 0 01 0 13 A N 10 75 0 04 10 66 0 05 0 09 0 12 STEV AME C P205 96 10 06 0 03 10 05 0 04 0 01 0 09 W K20 13 58 0 05 13 59 0 04 0 01 0 14 C MgO 3 36 0 02 3 28 0 02 0 08 0 07 C MnO 9 0 39 0 004 0 403 0 003 0 004 0 009 C BzO 9 0 210 0 002 0209 0 002 0 001 0 005 B A N 8 29 0 03 8 38 0 03 0 09 0 09 AL S P205 8 10 0 02 8 10 0 01 0 00 0 05 W PzOs 6 97 0 01 7 00 0 02 0 03 0 05 W K20 7 8 80 0 06 8 85 0 04 0 05
147. 2013 1 7 4 75 1 0E 01 1 0E 02 1 0E 03 A 1 0E 04 KE CM pm 1 0E 05 A Q Z 1 0E 06 1 0E 07 1 0E 08 1 0E 09 l 1 0E 08 1 0E 06 1 0E 04 1 0E 02 1 0E 00 Median 1 NIOR Horwitz HSD x Mois Bo AN x C P205 o W P205 e W K20 o C MgO B W MgO C MnO C B203 T As T Cd m S SiO2 A AL CMgO Horwitz Horwiz x2 Horwitz x0 5 76 Vol 7 2014 35 1 2006 2013 MER Ris ied 2s ar d d Ew 6 s La gt mg kg Mois 2006 147 1 70 0 30 17 7 4 78 0 06 2007 146 4 99 0
148. 1 250 mL 65 C 20 g L 150 mL 65 C2 10 60 3 2 1 25 mL 2 25 mL 200 mL 10 mL 15 mL 2 g 10 30 6 6 7 A 300 mL 200 mL EL 70 80
149. 1 mg mL K 9002 50 g 500 TI 50 g 1 1 200 mL JIS K 8580 immi LC JL 24 VI 1 500 g 1 000 mL JIS K 8576 CHET SAKE 5 g 3 E 140 Vol 7 2014 8 0 01 mg mL 1 mgmL 100 Lye 9 4 W Mo 3 1 300 mL 30 440 30
150. 11 12 11 C MgO 2 0 wv 2 63 96 2 95 WRU 7 16 1 9 wv 2 1 w v 2 0 ww 0 05 Bul 151 2 0 w v 0 1 w v C MgO 8 7 S 6 2 5 2 O 4 H in 3 iH ft 2 1 0 1 9 2 0 2 1 w v 6 7 C MgO C MgO
151. 144 10 88 0 11 1 0 0 37 0 30 2009 125 6 37 0 12 1 9 0 62 0 19 2011 114 17 44 0 22 1 3 0 53 0 42 W P20s 2006 157 9 02 0 12 1 3 0 46 0 26 2007 143 7 02 0 23 3 2 1 08 0 21 2008 149 9 16 0 24 2 7 0 93 0 26 2009 144 4 57 0 08 1 8 0 56 0 15 2010 144 11 56 0 52 4 5 1 63 0 32 2011 133 14 51 0 19 1 3 0 50 0 38 2012 131 2 86 0 06 2 1 0 61 0 10 2013 134 12 09 0 38 3 1 1 14 0 33 C K20 2011 122 10 41 0 23 22 0 79 0 29 W K20 2006 156 12 38 0 22 1 8 0 64 0 34 2007 145 8 43 0 15 1 8 0 61 0 24 2008 147 11 39 0 15 1 3 0 47 0 32 2009 145 8 35 0 13 1 5 0 52 0 24 2010 142 14 72 0 17 12 0 44 0 38 2011 132 10 17 0 17 1 7 0 59 0 29 2012 131 2 43 0 06 2 4 0 68 0 09 2013 132 11 74 0 35 3 0 1 08 0 32 2013
152. 30 40 30 C1 C 1 3 10 mL TK 100 mL X 1 4 1 3 ERE RSD o HorRat 2007 2012 Median RSD 2 Horwitz 13 AMEE TE O38 Median NIQR Honwitz SD HSD 500 um
153. ZH JIS K 8088 2011 CORR rt 2 1 4 a b c d 500 um
154. mz 146 E MS m z 161 m 195 PD 2 2 2 1 S uL LC MS MS SRM LC MS MS 5 0 5 ng mL 100 ng mL 0 0025 ng 0 5 ng Fig 2 0 999 120 999 20000 4 15000 4 10000 4 Response 5000
155. 0 05 2 C kD ul A zm mg 2013 nu SI im 3 4 1 2 X 2 y 7 8 b b 9 5 Sb 10 10 10 mon mon mon mon A T N 22 0 14 70 0 0079 14 88 0 11 0 004 0 009 A N 22 0 10 75 0 0012 10 72 0 10 0 004 0 010 C P205 22 0 10 06 0 0028 10 12 0 03 0 001 0 003 W K20 22 0 13 58 0 0015 13 55 0 15 0 006 0 015 C MgO 22 0 3 36 0 0025 3 30 0 03 0 0010 0 0027 C MnO 22 0 0 399 0 0000 0 399 0 011 0 0004 0 0010 C B203 22 0 0 210 0 0002 0 206 0 004 0 0001 0 0004 B A N 22 0 829 0 0000 8 34 0 09 0 004 0 010 S PzOs 22 0 8 10 0 0022 8 05 0 05 0 002 0 005 W P20s 22
156. 105 30 Table 1 Scheme 1 23 Table 1 Analytical conditions for total nitrogen and total carbon analyzer Combustion gas Highly pure oxygen purity no less than 99 99 v v Carrier gas Highly pure helium purity no less than 99 99 v v Combustion temperature Reaction furnace temperature 870 C Separation type Separation column Detector Thermal conductivity detector 0 05 g analytical sample lt Cover the sample with 0 2 g of sea sand and add a few drop of water lt Add 0 7 mL of hydrochloric acid 3 mol L drop by drop Weigh to the order of 0 1 mg into a combustion vessel
157. 0 1 EE HLZ 44 Vol 7 2014 7235 0 1 mol L HCI Cd 1 g 0 1 mol L 50 mL 1 1 mol L pH7 0 1 mol L pH7 0 Cd 1 g 1 mol L pH7 0 50 mL 1 ICP Table 2 Table 3 Table 1 Characteristics of soil used in this study Unit year APY 1 AP 2 SP 1 Ssp 2 pH E50 2009 6 6 1 6 2 6 2 2012 6 2 6 3 6 2 6 3 Ec mS m 2009 10 0 10 3 14 0 11 6 2012 16 6 16 9 15 6 13 4 Total nitrogen 9 2012 0 42 0 43 0 38 0 38 Total carbon 9 2012 5 8 5 8 5 4 5 5 Phosphate absorption coefficient mg 100g dry soil 2012 2370 2380 2360 2420 Available phosphate 2 mg
158. 99 96 DrEhrenstorfer GmbH 98 10 mg 100 mL 1 mL 100 ug 1 1 000 1 mL 0 5 1 000 ng 2 LC MS 3 4 3 1 LC MS MS Waters Quattro Premier XE Waters ACQUITY UPLC HSS C18 2 1 mm 100 mm 1 8 um 2 iuchi AW 1 3 KOKUSAN H 26F 4 BUCHI R 200 5 Waters Oasi
159. BORE 2008 lt http www maff go jp j syouan nouan kome k_hiryo odei_hiryo pdf 03_datal pdf gt 7 E 38 Bet 20 9 p 20 2008 EJERE 65 lt http www pref chiba lg jp ninaite network h2 1 fukyuu documents kakakukoutou pdf gt 8 18 1 p 110 2006 lt http www pref tochigi lg jp g04 work nougyou keiei gijyutsu sehikijun html gt 9 lt http www aic pref gunma jp agricultural management technology soil 01 index html gt 10 183 1991 11 20 10 16 lt http www maff go jp j seisan kanky
160. n a bLv o cu Lm E 11 TCd 65 57 9 D2 21 26 D2 1 8 ICP 3 11 3 07 mg kg Median 3 02 mg kg 82 NIQR 0 24 mg kg HSD 0 41 mg kg 14 9 3 D2 4 1CP 1 ICP ICP
161. 0 004 96 0 001 4 W Fe 0 001 0 0004 96 0 0002 5 W Fe 0 240 NIQR 0 013 5 4 1 5 Fe W Fe 7 amp 5 WwW
162. BEL 9 1 C B2O3 104 95 H 8 ICP 1 oO x e 0 460 0 480 0 490 0 500 0 510 0 520 0 530 0 540 0 550 0 560 0 561 ES 3 8 mE 3 9 3 0 012 10 TAs 52 29 17 6 Gz 0 248 amp Median 0 246 89 NIQR 0 014 HSD v yp E 7 7 H H 1CP
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164. pi H B Ibil lt Sp X fossn gt A B 3 4 F2 n 3 bi Y X Y a m i 1 i 1 e d f Spi A g lt Sp X toosn 2 b1 2 Sp X toosn 2 xj Xx Xi yi y b bo s PRIOR y 90 sp to 95 n 2 t
165. EDTA D S CaO 4 5 1 2 E S MgO 4 6 2 E 4 5 2 3 E 14 lt C MgO 4 2 1 C d 4 6 1 EDTA D b 4 6 2 E ff a Paani 4 1 1 z Median
166. 10 2013 10 Year 2009 2009 2010 2010 2011 2011 2012 2012 2013 Table 11 The yield of each crop body of 2009 to 2013 fresh weight Ap SP 5 i el eolit Season Test crops Part Fresh weight Fresh weight amid ere 4 kg plot kg plot kgiplo dex OF AP Summer Carrot Root 18 0 0 1 179 1 0 101 Leaf 10 5 0 4 9 6 0 9 109 Total 28 5 0 4 27 6 1 8 16 104 Winter Spinach Edible portion 13 7 0 8 18 6 1 0 8 74 Summer Spinach Edible portion 4 5 0 1 5 8 0 6 4 77 Winter Qing geng cai Edible portion 22 4 0 7 26 9 0 8 12 83 Summer Turnip Root 8 9 0 6 9 4 0 9 95 Leaf 8 7 1 0 10 0 1 3 88 Total 17 6 1 5 19 3 22 16 91 Winter Spinach Edible portion 8 1 0 0 10 3 0 5 8 79 Summer Carrot Root 12 3 0 5 12 1 0 2 101 Leaf 10 0 0 6 9 7 0 8 103 Total 22 3 0 1 21 8 0 5 14 102 Winter Spinach Edible portion 11 3 0 5 13 3 0 6 8 85 Summer Carrot Root 12 2 0 9 10 3 1 4 118 Leaf 5 4 0 3 4 6 0 6 119 Total 17 6 1 14 9 2 0 14 118 1 Sludge fertilizer application plot 2 Standard plot 3 This value is shown in the recommending rate of fertilizer application local governmen
167. 2008 2 4 2011 5 68 89 2012 2009 3 73 94 2010 2010 2012 E 6 61 83 2013 1 152 97 115 pa 85 106 rin 130 Vol 7 2014 Verification of Performance Characteristics of Testing Method for Soluble Silicic Acid in Fertilizer by Potassium Fluoride Method Yasushi MIYASHITA Food and Agricultural Materials Inspection Center Nagoya Regional Center Now Ministry of Agriculture Forestry and Fisheries Tokai Regional Agricultural Administration Office Food Safety and Consumer Division We verified performance characteristic of testing method for hydrochloric acid soluble silicic acid S S1O by potassium fluoride method described in Testing Method for Fertilizers The accuracy of testing method for S SiO was assured from 3 replicate determinations of 3 fertilizer samples containing 10 40 96 S S1O which were prepared each test As a result the mean recoveries ranged from 98 4 101 0 On the basis of 7 replicate measurements of testing method the limit of quantitative value LOQ was estimated at 0 3 96 Reported in Research Report of Fertilizer median normalized interquartile range
168. NEN 0 6 2 2 2 V be nel 3 4 5 6 7 pur ue P E0223 Wo HE mr C P20s 10 20 76 0 12 0 6 0 10 0 15 0 7 2 48 CMnO 10 0 519 0 011 2 2 0 0 011 2 2 0 58 C MgO 10 3 76 0 02 0 6 0 01 0 02 0 6 1 23 1 x2 2 3 4 5 6 Sbir V Sob Sr 7 8 9 F 9 10 0 05 23 02 2 4 2 1 2 z 3 C MnO 77 A N 100
169. 1g 100 mL 0 1 0 2 mol L Scheme 1 4 IUPAC 10 2 3 5 10 3
170. Mo 5 Mo mew PMS sone MRR MERE awa 1 p 95 c 95 5 E 96 F 25 G9 96 W Mo Mo 2 5 2 5 2 51 0 01 0 2 100 2 0 01 0 4 Mo 0 1 0 1 0 101 0 001 0 8 100 8 0 002 1 6 1 Mo 2 3 3 4 C B A 5 D C A x100 6 E B A X100 7 3 8 G E B x100 3 2 7 W Mo 6 Lic x10 x2xt n 1 0 05 Were 142 Vol 7 2014 Mo 0 02 0 006 AOAC 85 110 Mo 0 02 W Mo
171. VEL 1 mI FR C FAMIC E etai n un E ELESIV CVS HO J ISO IEC Guide 31 gt n E d ISO IEC Guide 35 AD kd x 34x EFL B
172. de 2011 100 6 P5 Fix 100 m EJE 6 0 amp 3 JE PRD B EE 2009 at 9 2013 3 8 HE MA H
173. nu 2 1 500 um 3 5 T
174. 102 Vol 7 2014 6 sw se 56 56 HbO 1 43 0 14 0 07 0 22 9 T N 14 83 0 09 0 06 0 14 8 A N 10 36 0 13 0 07 0 21 9 C P2O5 10 79 0 03 0 08 0 09 10 W KO 13 07 0 08 0 10 0 16 10 C MgO 3 18 0 08 0 04 0 12 9 C MnO 0 356 0 009 0 012 0 018 10 lt PAPELED 38 C BrOs 0 203 0 005 0 004 0 009 10 1 2 4 2 5 3 6 5 FAMIC A 10 2 6 4 6 A FAMIC A 10 A 4 2018 6
175. 7 420 nm 0 234 abs 100 mL P Os mg 400 nm 0 38 abs 100 mL P gt Os mg NIQR 0 006 abs 100 mL P2Os mg 0 014 abs 100 mL P20s mg 7 lt NIQR 420 83 5 6 0 234 0 006 415 7 1 14 0 258 0 012 410 18 5 28 0 298 0 012 400 6 2 33 0 385 0 014 5 0 0 1 abs 100 mL P205 mg 90 Vol 7 2014
176. 8 C MnO 115 102 9 ICP 4 3 8 0 517 Median 0 513 77 NIQR 0 014 HSD Zs 2013 E 85 0 023 10 12 10 ICP 2 ICP HE 5 5 eS 3 7
177. z Visas ROR u D EFEO 4m 0 08 0 01 Ap 0 15 mg kg 4338 3 28 96 2 E 6 04 mg kg mG 2013 YEA OBA Lu nan nul 119 2 0 03 mg kg G lumeas h 5424500 i Umeas d E zs Uca 24cm AD Ymeas Am Ucrm Umeas sq FRR eta sr UC Am Am Uses UcrM E y UC Am V meas UcRM x Ck Am S Ucan m u Ussy
178. zu F2 tet HOEY FAMIC m3 E IZ EM E E a 4 h 2 i ucgy KU G jvc Hf E E FOS 35 COD EE EDS umea 5 DS ucap k 2 HUTHE 5 Am Uca m A 7 B 9 16 14 Am Ucan 2 SRH Y
179. 0 20 40 60 80 100 0 20 40 60 80 100 ng mL ng mL Fig 2 Calibration curves of Aminopyralid and Picloram by their derivative peak areas in selected reaction monitoring chromatograms 3 APSE HERE 2 2 1 5 uL LC MS MS oo oy 4 50 pg kg 2 4 3 2 0 0025 w v 9 1 20mL 4 mL Table 3 HELO mL 4 mL 6
180. 15 cm CHLI 9 20 cm 10 26 11 13 11 29 2 4 6 2013 3 6 CE 1 m 3 ip rpm 0 5 g Multiwave 3000 Perkin Elmar 50 mL ICPM 8300 6
181. 2013 91 10 RE aT 5 7 33 1 3 32 4 13 7 0 0 58 8 14 1 2 i OO O O OO O oo QRQNQOmW c cd edo do Bd cd oed ed Bd c eu ud 5 FAMIC A 10 2013 11 143 3 82
182. 9 PRSDR Horwitz 9 HorRats 1 2 5 ao sw sg y 9 dii m Ko o eo a tomy orate HO 9 1 43 0 07 0 22 15 1 3 8 3 99 T N 8 14 83 0 06 0 14 0 9 23 0 35 A N 9 10 36 0 07 0 21 2 0 2 8 0 71 C PzOs 10 10 79 0 08 0 09 0 8 2 8 0 29 W K20 10 13 07 0 10 0 16 1 2 2 7 0 45 lt E E C MgO 9 3 18 0 04 0 12 3 8 3 4 1 13 C MnO 10 0 356 0 012 0 018 4 9 4 7 1 06 C BO 10 0 203 0 004 0 009 4 7 5 1 0 92 1 5 2 x 3 6 x 7 HorRat 3 8 4
183. B i i11 AEST ET ts A N 4 1 2 a C YEMEN Ji S P 4 2 2 ae Be AS Pas a Suid j W P 4 2 4 4 W 205 a 1 RNE ie LH W KO 4 3 3 a jan As 5 2 a Cd 5 3 a Hg 5 1 a Ni 5 4 a 43 Pb 5 6 a 2A 108 Vol 7 2014 2C C
184. TVR ROOKIE JE 2014 EI AD FAMIC A 13 ISO Guide 31 2000 JIS Q 0031 2002 E 4 A T 5 EHE Lu no m Lu ies ii a n El HE 3 ES 2013 FAMIC A 13 103
185. po mm TUE 9 Lv ame EDTA 13 AL 78 59 15 ARED EDTA 4 ICP 88 Vol 7 2014 4 2 36 78 Median 36 79 88 NIQR 0 95 HSD 0 61 4 3 EDTA 1 2 EDTA EDTA EDTA
186. 3 4 13 1 a PIN f U 7 8 3 5 A EOD 1 4 R 4 1 133 2 50 g 250 mL lt 200 mL 30 40 30 1 5 25 mL 3 Wie Tr N Oo 3 X1 3 1 EDTA EDTA 3 RER 4 100 5 min 98 0 96 0 49
187. 4 2 11 6 96 0 0346 1 60 2 3 6 9 0 188 1 10 6 5 9677 6 w 0 105 1 15 6 8 13 2 0 0345 16 1 0 0365 18 3 25 3 25
188. 6 10 ug kg 5 ug kg 2013 5T H X 1 2 Health and Safety Executive Aminopyralid Results of Analysis of Contaminated Manure Soil and Damaged Crops lt http www pesticides gov uk guidance industries pesticides topics using pesticides General aminopyralid results of analysis of contaminated manure soil and damaged crops gt 3 TIAN Yingying LIU Xing
189. HFBUEOS HER TE E fri 1 15 96 d 2 9 9674 8 96 ux 7238 ZEA 0 0015 16 1 4 izE X 6 8 13 2 D 18 3 HPLC 17 S
190. ISO IEC 17025 2005 JIS Q 17023 2006 FAMIC A B 38 C 14 1A 1C u sw sg a b c CORR A B C
191. 2010 4 85 106 2011 8 BEEZ 2011 EE 5 68 89 2012 9 2012 6 61 83 2013 10 FAMIC lt http www famic go jp ffis fert sub9 html gt ToS 5 K F 11 Horwitz W Kamps L R Boyer K W Quality control Quality assurance in the analysis of foods for trace constituents J AOAC Int 63 6 1344 1354 1980 12 Thompson M Recent Trends
192. 68 3 75 0 11 3 1 0 93 0 12 1 4 HorRat 2 Horwitz 3 6 T As T Cd mg kg 3 z 2 1 2 7 tk UN z gt 10 C P205 amp W P505 C MgO 1 C P205 C MgO
193. 128 20 60 0 19 0 9 0 43 0 45 W P200s 133 12 08 0 39 3 2 1 16 0 33 W K20 57 11 72 0 39 33 1 19 0 32 65 11 81 0 33 2 8 1 00 0 33 C MgO 116 6 17 0 13 2 1 0 69 0 19 ICP 9 6 22 0 10 1 5 0 51 0 19 W MgO 109 3 80 0 63 16 6 5 07 0 12 ICP 7 3 06 0 86 28 1 8 31 0 10 C MnO 102 0 513 0 013 2 5 0 56 0 023 ICP 9 0 519 0 030 5 9 1 33 0 023 C B203 95 0 247 0 014 5 6 1 12 0 012 ICP 8 0 243 0 005 2 0 0 40 0 012 T As 29 10 13 0 90 8 9 0 79 1 14 17 10 49 0 63 6 0 0 53 1 18 T Cd 9 3 20 0 39 12 3 0 91 0 43 D2 21 3 11 0 51 16 4 1 22 0 42 26 3 02 0 11 3 7 0 27 0 41 ICP 8 2 70 0 14 54 0 39 0 37 S SiO 46 35 14 0 55 1 6 0 93 0 59 11 35 50 0 70 2 0 1 18 0 60 AL EDTA 15 37 30 1 01 2 7 1 66 0 61 59 36 56 0 86 24 1 42 0 60 S CaO 59 30 06 0 65 2 2 1 18 0 55 S MgO 59 4 62 0 15 3 2 1 01 0 15 C MgO EDTA 7 3 86 1 35 34 9 10 68 0 13
194. 7 9 2 5 2 JIS Z 8402 2 1999 Grubbs Cochran f amp Bx 387003 x 5 B Fr fRI ud FSS 4 5 06 2 DF 1 RER 4 3 ISO 5725 2 1994 327v Cochran 98 Vol 7 2014 2 2 23 2 6 D us TES mere TOSS x s i5 023 06 5 HbO 10 0 1 62 0 07 4 5 0 04 0 08 5 1 1 56 ERLE T N 10 0 14 90 0 23 1 5 0
195. DES Fe 0 001 Fe 0 01 0 004 0 001 Fe 0 001 0 0004 96 0 0002 135 6 kis doe o 9 95 W Fe Fe 0 01 0 01 0 0099 99 5 0 0004 0 004 0 001 W Fe Fe 0 001 0 001 0 00108 108 2 0 00004 0 0004 0 0002 1 Fe 2 3 7 4 x100 x10 6 x2xt n 1 0 05 7 8 4
196. ao amp 6 S SiO gt 2 2 1 98 0 03 0 3 0 1 1 S SiO2 OF At 2 7 3 x10 4 X2 t n 1 0 05 4 1 19 7 NIQR NIQR S SiO 28 25 36 15 WT
197. Vol 7 2014 AP Sludge fertilizer application plot lm 2m lm Fig 1 Plot plan of the test field SP Standard plot Table 4 The design of the test plots Amont of application g lt Sludge fertilizer application plot AP Sludge fertilizer Ammonium sulfate Ammonium dihydrogenphosphate Potassium chloride Fused magnesium phosphate Total Standard plot SP Sludge fertilizer Ammonium sulfate Ammonium dihydrogenphosphate Potassium chloride Fused magnesium phosphate Total 1 Content as P205 2 Content as KO 2000 285 103 200 283 170 114 200 N g 66 60 126 60 20 80 2m 2m p g 104 40 144 104 40 144 The applied components K g 65 72 72 72 Cd mg 7 3 47 4 KU 2012 10 22 12 kg
198. 1H 4 6 Zu 1 m 50 Vol 7 2014 65 24 6 CC 24 1 mm 500 pm ZM200 Retsch 6 000 rpm 2 6 2 D 6 3 44 m 1 2012 2012 10 26 2013 3 6 A 1 4
199. 23 C 2 60 11 7 20 0 84 0 62 150 Vol 7 2014 C MgO 5 C MgO 11 11 L 1 3 2 C MgO 6 11 11 C MgO 2 87 2 56
200. FE ZO CHE 0 1 mol L HCl Cd 0 1 mol L HCLCd amp tki BRL CLV B lt OD fF TER RODA RU DIRE LAB DSLR ESI TWH 1 mol L HEZ pH 7 0 Cd 1 mol L pH 7 0 1 mol L MEZ pH 7 0 Cu Zn 0 1 mol L 50 mL 30 1 0 1 mol L HCI Cd 10 g ICP FO 1 mol L pH 7 0 Cd Cu Zn 2
201. Fig 7 Changes of the 2009 2013 year of the quantity of cadmium load by fertilizer 2013 2013 VEN quantity of cadmium accumulation to the soil and the 0 1 mol L HCI Cd density 5 EE 2009 2 2012 E EEO 0 1 mol L HCI Cd 1 mol L BE pH 7 0 Cd 0 05 2012 4 E EE 0 05 64 Vol 7 2014 2013 gt 0 05
202. IlzI 2 2 lt lz 3 Il 3 3 Mean 4 OMedian 5 NIQR Median O s 2 E d Oss 2XNIOR VN d 6 7 NIQR NIQR SD 8 Horwitz s 8 e g 3X KO Horwitz SD HSD C 1 0 01 HSD 0 01 x C93 0 138 C saule HSD 0 02 x C 8495 1 2 X 107 SC 0 138 set HSD 0 22 XC C lt 1 2X 107 72 Vol 7 2014 9 RSD h RSD NIQR Median x100 b 10 HorRatyop FX
203. Table 7 11 28 kg 13 33 kg gt 0 05 0 56 mg kg 0 47 mg kg THV 0 05 0 75 mg Table 7 Cadmium uptake and yield of spinach in the test Part Unit Test plot 1 Test plot 2 Average t test lt Sludge fertilizer application plot AP Fresh weight edible portion kg 10 95 11 60 11 28 ns Dry weight edible portion kg 1 30 1 41 1 36 n s Cadmium concentration edible portion mg kg 0 57 0 58 0 53 0 54 0 56 significance Quantity of cadmium uptake edible portion mg plot 0 74 0 75 0 75 0 77 0 75 n s lt Standard plot SP gt Fresh weight edible portion kg 13 75 12 90 13 33 Dry weight edible portion kg 1 67 1 53 1 60 Cadmium concentration edible portion mg kg 0 49 0 49 0 46 0 43 0 47 Quantity of cadmium uptake edible portion mg plot 0 83 0 81 0 70 0 66 0 75 1 Content in the drying soil 2 Quantity of cadmium uptake Harvest dry weight x Cadmium concent
204. 0 0354 0 0345 0 0374 BU 0 0365 0 0042 0 0031 0 0014 0 0015 Fig 1
205. a IQR imi 2013 71 E IOR a NIQR b NIQR NIQR IQR X 0 7413 b z 2 c lt Gu O Median z xi Median NIQR o 2 z ISO IEC 17043 JIS Q 17043 z lzIS2 te 2 lt lzl 3 ll 3 2 1 N 2 z
206. ee HAAA H Hr 2 HPLC PPM f 1 een ere err Te are eRe ere eT PEE pU eee 4 EUER a da eis Sq eique T Pret Sb din va EUN e 5 lt JA gt alli 6 SERENE ee es BAEZA lt gt 7 2013 FE 3 8 2013
207. pH 55 pH 75 n Sludge fertilizer application plot AP 7 0 Standard plot SP y m a 6 0 z 5 5 5 0 Carrot Spinach Spinach Qinggengcai Turnip Spinach Carrot Spinach Carrot Examination After summer After winter After summer After winter After summer After winter After summer After winter After summer start cultivation cultivation cultivation cultivation cultivation cultivation cultivation cultivation cultivation 2009 2009 2009 2010 2010 2011 2011 2012 2012 2013 Fig 2 Changes of the pH of cultivated soil 3 0 1 mol L HCI Cd 0 1 mol L HCI Cd Table 12 Fig 3 0 1 mol L HCI Cd 6 0 1 mol L HCI Cd 5 Table 12 2013
208. 29 B 300 mL 50 mL 15 mL 300 mL Bb Ebl c f 100 g L 100 g L 2 mL Lic C 300 mL BK CY 2 E 20 mL 1 2 KK 5 mL 1 mL 120 C 1 800 C 2 0 1 mg Zs
209. A NIQR p 96 2 0 60 0 87 0 49 0 62 0 57 0 75 0 48 RS Drob 4 C 90 1 8 3 1 1 5 1 9 1 7 2 4 1 3 PRSD D 95 1 7 1 9 1 7 1 7 1 7 1 8 1 7 S SiO gt A 1 S Si02 10 40 0 66 0 13 2 S SiO gt 2 0 3 0 1 3 1 3 3 1 28 25 36 15 NTQR I M 98 4 101 0 H HORR S Si02 13 0 48 0 87 COD SR P HorRat p 1 03 1 63 0 85 1 09 0 98 1 35 0 80
210. BUE 17 2 7 BA EERTE 2013 81 Er z g 5 XU bn Q 30 20 10 0 10 20 30 20 10 0 10 20 C MgO S CaO X2 5 x 2 6 C MgO z S MsO S CaO z e z e z Z Z 20 10 S MgO e 10 20 10 0 10 20 C MgO 2 7 S MgO C MgO z e z 6 4 D Mois 136
211. HorRat 1 3 0 67 1 4 0 82 2 0 1 09 1 4 0 81 1 3 0 53 8 2 3 10 1 3 2 0 m H 41 x 1
212. NIQR 0 48 0 87 96 1 3 3 1 S SiO gt HorRat 0 80 1 63 AOAC 100 10 2 3 S SiO 128 Vol 7 2014 7 E E E R RR TAE S SiO2 2006 66 33 92 2007 67 28 25 2008 68 33 35 2009 69 32 67 2010 67 33 52 2011 59 30 69 2012 67 36 15 D 2 3 NIQR 4 C B A x100 5 Horwitz 6 HorRat CD 4
213. S SiO gt JIS 1 WA S SiO JIS K8885 1 En S Si0 gt 1 S SiO en 212 um S SiO gt 2 S SiO gt 2 40 SL
214. pot 4 EDTA e ee DM 2A fel WATE 2 m ME Sob E 3 EDT A III 13 26 13 33 0 07 100 5 0 49 1 EDTA amp K III DEK Fe 2 3 3 x100 we 4 2 3 W Fe 5 Fe W Fe
215. 3 50 ug kg 0 0025 w v 9 1 0 mL 4 mL 4 50 ng mL 50 ng mL 5 2 2 1 40 ug kg 400 ug kg 1 000 ug kg 71 2 M 117 6 96 RSD 10 7
216. 3 1 2 88 Median 2 93 99 NIQR 0 84 HSD 0 10 2006 2011 FED X 82 Vol 7 2014 NIQR 0 12 0 41 HSD 0 04 0 16 NIQR 3 2
217. 58 Vol 7 2014 1 mol L pH 7 0 Cu KU Zn 6 pH 7 0 Cu Zn 2009 LH d gt 0 05 2011 H HZ ARI LFA TE Sd OMEN 22 1molLB pH 5 gt gt 1 mol L f 1 102 O 7 9
218. lt 11 11 x 11 11 2 7 2 C MgO 09 11 10 12 100 2 212 um 09 11 3
219. lt Add 0 2 mL of water and shake the vessel calmly to mix the sample completely with the solution 100 C for 90 minutes 105 C for 30 minutes Measurement by total nitrogen and total carbon analyzer Scheme 1 Flow sheet for organic carbon in sludge fertilizer and compost by combustion method 4 IUPAC ISO AOAC 10 2 3 5 9 BRE OME FAL WEE AIAN 10 3 f P 1
220. 0 01 0 01 0 15 0 16 n s 0 01 0 01 0 68 0 58 signifi 0 02 0 05 cance 0 32 0 30 n s 0 01 0 02 0 41 0 38 n s 0 005 0 04 0 73 0 68 n s 0 02 0 06 0 75 0 75 n s 0 01 0 08 0 22 0 17 signifi 0 02 0 004 cance 0 24 0 18 signifi 0 01 0 01 cance 0 46 0 34 signifi 0 03 0 01 cance 5 42 5 53 n s 0 07 0 13 5 It is no significantly different for processing examination section t test 5 of both sides levels of significance n 4 2x2 repetition x number of samples 6 It is significantly different for processing examination section t test 5 of both sides levels of significance n 4 2x2 repetition x number of samples 62 Vol 7 2014 7 RRHUIEM OE EE Table 16 f m 15 cm 0 67 4 5 53 mg
221. 09 11 C MgO 0 2 23 2 93 O 0 39 C MgO C MgO eu N 4 6 4 C MgO 09 10 lt 11 12 11 4 BE FEDS C MgO 12 11 2 C MgO 5 30C 2 C MgO 4 1 c FAVOR RECO C x1 C
222. 2010 2010 2011 2011 2012 2012 2013 Table 15 Absorption and the amount of cadmium concentration of each crops in 2009 2013 1 Cadmium Concentration 2 Season Test crops Part AP sp t test mg kg mg kg Summer Carrot Root 0 12 0 11 nz 0 01 0 02 Leaf 0 24 0 22 n s 0 02 0 02 Total Winter Spinach Edible portion 0 62 0 61 n s 0 01 0 02 Summer Spinach Edible portion 1 40 1 56 n s 0 10 0 07 Winter Qing geng Edible portion 0 20 0 17 signifi cai 0 01 0 01 cance Summer Turnip Root 0 08 0 08 n s 0 01 0 002 Leaf 0 16 0 17 n s 0 01 0 01 Total Winter Spinach Edible portion 0 53 0 36 signifi 0 01 0 02 cance Summer Carrot Root 0 24 0 23 n s 0 01 0 01 Leaf 0 31 0 29 n s 0 01 0 02 Total Winter Spinach Edible portion 0 56 0 47 signifi 0 02 0 03 cance Summer Carrot Root 0 18 0 15 n s 0 02 0 02 Leaf 0 33 0 28 signifi 0 02 0 03 cance Total The sum total 1 Content in the drying soil 2 Sludge fertilizer application plot 3 Standard plot 4 Standard deviation n 4 2x2 repetition x number of samples Quantity of cadmium uptake 2 AP sp t test mg plot mg plot 0 21 0 20 n s 0 02 0 03 0 32 0 31 n s 0 02 0 01 0 54 0 50 n s 0 03 0 04 1 18 1 34 signifi 0 004 0 02 cance 0 72 0 96 signifi 0 04 0 01 cance 0 21 0 21 n s 0 01 0 01 0 04 0 04 n s 0 003 0 00 0 10 0 11 n s
223. 4 ave Mean Median Usa s NIQR HsD RSD HorRatrob mg kg mg kg mg kg mg kg mg kg mg kg Mois 2 88 2 93 0 14 0 70 0 84 0 10 28 7 8 42 A N 9 87 9 92 0 13 0 55 0 74 0 28 7 5 2 63 C P20s 20 64 20 60 0 04 1 21 0 20 0 45 1 0 0 44 W P20s 12 05 12 09 0 07 0 53 0 38 0 33 3 1 1 14 W K2O 11 70 11 74 0 06 0 62 0 35 0 32 3 0 1 08 C MgO 6 19 6 18 0 02 0 51 0 13 0 19 2 2 0 71 W MgO 3 75 3 79 0 12 0 60 0 68 0 12 18 0 5 50 C MnO 0 517 0 513 0 003 0 067 0 014 0 023 2 8 0 64 C B203 0 248 0 246 0 003 0 033 0 014 0 012 56 1 11 T As 10 22 10 31 0 27 1 16 0 99 1 16 9 6 0 85 T Cd 3 07 3 02 0 06 0 46 0 24 0 41 8 1 0 60 S SiO gt 35 15 35 18 0 14 0 71 0 55 0 59 1 6 0 92 AL 36 78 36 79 0 21 1 23 0 95 0 61 2 6 1 56 S CaO 30 19 30 09 0 18 0 90 0 70 0 55 2 3 1 27 S MgO 4 59 4 62 0 04 0 29 0 16 0 15 3 4 1 06 C MgO 3 88 3 77 0 03 0 67 0 14 0 12 3 6 1 11 1 2 3 4 5 6 Horwitz 7 8 HorRat 9 T As T Cd mg kg
224. 5 cm 2 HH E 2013 10 22 12 kg 2012 5 4 8 2 mg 100 g iE 10 mg 100g K g 73 80 80 80 Cd mg 7 3 0 0 E
225. Average t test lt Sludge fertilizer application plot AP gt 0 20 0 19 0 038 0 036 6 1 15 1 0 1 mol L HCLCd mg kg Exchangeable Cd pH HO EC mS m 0 15 0 16 0 030 0 029 6 0 16 3 0 1 mol L HCLCd Exchangeable Cd pH BBO EC mg kg mS m 0 20 0 20 0 039 0 038 0 20 0 038 PES 5 significance significance 6 2 16 8 lt Standard plot SP gt 0 17 0 17 0 032 0 031 6 1 0 16 0 031 16 7 1 Content of cadmium dissolved with 0 1 mol L hydrochloric acid in the drying soil 2 Content of cadmium dissolved with pH 7 0 1 mol L ammonium acetate solution in the drying soil 3 Soil pH determined on 1 5 soil water suspensions with a glass electrode n 2 4 Soil electrical conductivity determined on 1 5 soil water suspensions with an electrical conductivity meter n 2 5 It is significantly different for standard plot t test 5 of both sides levels of significance n 4 2x2 repetition x number of samples 4 1 2009 2009 5 EH D Table 11
226. Fe 10 Fe 0 5 Fe 0 05 101 1 107 0 Fe 10 Fe 0 5 Fe 0 05 1 1 7 0 Fe 1 Fe 0 1 Fe 0 01 103 6 105 7 Fe 1 Fe 0 1 Fe 0 01 3 6 5 7 134 Vol 7 2014 W Fe AOAC 10 95 967 102 96 0 1 90 108 0 01 WT 85 110 W Fe
227. HL7 2 L Hv 1 2012 2012 10 A 26 2013 3 6 1 i ELE za AS AE I vel ive 16 4 HIM pH EC mol L HCI Cd Table 1 2 He 1 a 4 j 4 ET th er 4 ALTT 3 M E HE D AS PA D Ea 5 I Lu ETA Zs HR ER E
228. PH BIZ Se KR FAB 7 2 1 TEL 050 3797 1856 FAX 048 601 1179 http www famic go jp 26 12 7 11 TEL 03 3260 4767 amp
229. c j PBL WRT OOELL ISO Guide 35 2006 JIS Q 0035 2008 ISO Guide 31 2000 Q 0031 2002 2013 10 1 I ARO ARB BH CH BC 2 A ARS TI nr 10 6 EE gt A FAMIC A 13
230. 1 1590 EE ERRO E 2 1 1 7 zI aw 2 EL H 3 0 05 g 0 1 mg 40 60 70 65 CT 5 24 H 0 09 g 1 of E
231. 12 g ha 2011 0 1 mol L HCI Cd lt 0 05 1 7 mg 18 g ha 2011 BED 1 mol L pH 7 0 Zn 0 05 5 mg kg 1 2011 500 kg 10 a 2 1t 10 a 9
232. 35 30 25 20 RSD PRSD 1E 0 1E 1 1E 2 1E 3 1E 4 1E 5 1E 6 1E 7 Median g g 2 2007 2012 RSDs lt C MgO A FREE PRSDR PRSDRx2 PRSDRx0 5 ux p 1 C MgO TOS Median NIQR RSD Homat HSD 6 v 96 v 2007 86 3 17 0 21 6 6 1 95 0 11 2008 89 5 80 0 14 2 4 0 79 0 18 2009 87 2 34 0 20 8 7 2 48 0 08 2010 88 5 42 0 11 2 1 0 67 0 17 2011 78 3 36 0 23 6 8 2 05 0 11 2012 81 6 77 0 19 2 8 0 94 0 20 2011 128 2 48 0 07 2 8 0 81 0 09 1 4 HorRat 2 5 Horwitz 3 6 148
233. Ellison S L R Wood R The International Harmonized Protocol for the Proficiency Testing of Analytical Chemical Laboratories Pure amp Appl Chem 78 1 145 196 2006 5 1992 1992 6 Horwitz W Kamps L R Boyer K W Quality control Quality assurance in the analysis of foods for trace constituents J AOAC Int 63 6 1344 1354 1980 7 Thompson M Recent Trends in Inter laboratory Precision at ppb and sub ppb Concentrations in Relation to Fitness for Purpose Criteria in Proficiency Testing Analyst 125 385 386 2000 8 Horwitz W Albert R The Horwitz Ratio HorRat A Useful Index of Method Performance with Respect to Precision J AOAC Int 89 4 1095 1109 2006 9 AOAC OFFICIAL METHODS OF ANALYSIS Appendix D Guidelines for Collaborative Study Procedures To Validate Characteristics of a Method of Analysis AOAC INTERNATIONAL 2005 10 p 108 114 LEE 1988 93 2013 N Result of Proficiency Testing for Determination of Major Components and Harmful Elements in Ground
234. H EE 80 Vol 7 2014 2 3 4 30 20 10 of e 0 10 20 30 30 20 10 0 10 20 30 C P O 2 1 W P O C P O z e z 30 Z 20 10 0 C P 0 10 20 42 3 C MgO C P O z e z z 30 C B 03 30 20 10 X 30 20 10 0 10 20 30 C MnO 2 2 C B O C MnO z e z 30 X z 10 0 W MgO 20 10 20 30 2 4 C MsO W MgO z z
235. ISSN 1883 4981 7 2014 Research Report of Fertilizer Vol 7 2014 3 Food and Agricultural Materials Inspection Center Incorporated Administrative Agency Saitama Japan CX FAMIC
236. TCd 14 96 C MgO 13 4 2 3 10 Seated 4 Mean Median Mean Median 20134 EHE 73 SD NIQR NIQR HSD HSD X0 5 HSD X2 2006 2013 5 1 C 5 2 Mois 136 A N 136 C P20s 129 W P205 134 W K20 132 C MgO 129 W MgO 120 C MnO 115 C B203 104 T As 52 T Cd 65 S SiO gt 60 AL 78 S CaO 61 S MgO 61 C MgO 79 1 z IzlI 2
237. 10 Bul mar OOOO Or OQ CO O 0 0 OO QI 118 Vol 7 2014 4 2 NT 0 mg kg mg kg mg kg mon mg kg 5 ES x mg kg mg kg aon mu B As 22 0 2 38 0 0064 2 52 0 09 0 004 0 009 O Cd 22 0 5 89 0 0000 5 91 0 08 0 003 0 008 O Hg 22 0 0 89 0 0003 0 88 0 03 0 001 0 003 O Ni 22 0 45 6 0 0228 45 1 1 4 0 05 0 13 O Pb 22 0 247 0 0209 252 1 7 0 06 0 16 O C T Cu 7 3 581 0 5912 586 2 3 0 2 3 0 O T Zn 7 3 994 2 6378 975 5 8 0 6 7 4 As 7 3 21 0 0 1119 21 8 1 4 0 1 1 8 O Cd 7 3 1 82 0 0014 1 83 0 02 0 002 0 029 O Hg 7 3 0 46 0 0006 0 47 0 0000 0 00009 0 00119 Ni 7 3 75 6 0 3250 73 2 7 0 2 2 2 O Cr 7 3 79 3 0 1666 80 5 1 7 0 2 2 1 O Pb 7 3 36 0 0 0065 36 1
238. 9 2 H Ae HE ER OLE GUB MRE OT 20 ug kg 7 x10 x2xt n 1 0 05 ni LC MS MS 7SZE3IR NEZP33AO 10 ug kg 5 ug kg Table 6 Table 5 Accuracy result and repeatability precision Spiked level Clopyralid Aminopyralid Picloram Pape DO ES URSUS MU a ee S ug kg Recovery RSD Recovery RSD Recovery RSD 1 000 82 8 3 2 78 3 7 3 87 9 3 7 Cattle manure compost 1 400 114 2 1 2 104 5 3 7 117 6 1 5 40 95 7 2 6 83 0 3 4 75 5 5 7 1 000 82 3 3 3 80 8 4 0 84 4 2 7 Cattle manure compost 2 400 90 1 3 8 81 0 3 3 88 7 1 1 40 101 3 6 5 83 5 4 7 83 0 2 7 Composted sludge 1 000 819 49 8 6 87 900 24 fertilizer 400 111 2 2 5 94 6 4 4 97 1 2 8 containing cattle manure 1 40 865 107 71 2 2 6 827 9 2 Composted sludge 1 000 890 41 isi di 865 23 fertilizer 400 81 6 5 1 94 0 1 2 99 2 3 4 containing cattle manu
239. 96 96 96 96 Calcium cyanamide 1 10 0 1 07 0 01 1 2 0 0 01 1 2 0 67 Calcium cyanamide 2 10 0 0 404 0 011 2 8 0 0 011 2 8 0 76 d fertiliz taini Compound fertilizer contains dolo dre 25993 3 0 0 00 0 004 3 1 1 06 Calcium cyanamide Compound fertilizer 10 0 0 799 0 011 1 4 0 011 0 016 2 0 2 96 Ammonium sulfate 10 0 0 0374 0 0009 2 4 0 0011 0 0014 3 8 4 22 1 10 Refer to the footnote of Table 2 1 2 yl SAO Table 3 IUPAC 9 1 5 14 Vol 7 2014 1 REE 35 mmol L 4 1 78 22
240. Cattle manure compost Aminopyralid 50 101 5 100 8 Picloram 50 102 7 108 2 Clopyralid 50 105 6 106 6 Composted sludge fertilizer i Ni Aminopyralid 50 101 5 100 3 containing cattle manure Picloram 50 102 7 101 0 a Mean Value n 3 b Spiked standard in sample solution 6 2 2 40 ug kg 400 ug kg 1 000 ug kg EE 1 3 Table 5 74 7 967 114 2 96 71 2 M 104 5 72 7 117 6 96 7 RSD 1 2 10 7 RSD 1 1 10 2 RSD 1 1
241. D We RWE E 7 Horwitz W Protocol for the Design Conduct and Interpretation of Method Performance Studies Pure amp Appl Chem 67 2 331 343 1995 I ao 8 Thompson M R Ellison S Wood R The International Harmonized Protocol for the Proficiency Testing of Analytical Chemical Laboratories pure amp Appl Chem 78 1 145 196 2006 9 Thompson M Recent trends in inter laboratory precision at ppb and sub ppb concentrations in relation to fitness for purpose criteria in proficiency testing Analyst 125 385 386 2000 42 Vol 7 2014 Determination of Soluble Silicic Acid in Fertilizers Containing Silica Gel Fertilizer by Potassium Fluoride Method A Collaborative Study Shinji KAWAGUCHI and Akira SHIMIZU Food and Agricultural Materials Inspection Center Nagoya Regional Center Food and Agricultural Materials Inspection Center Nagoya Regional Center Now Fertilizer and Feed Inspection Department A collaborative study was conducted to evaluate the applicability of the method of potassium fluoride for determination of soluble silicic acid in fertilizers containing silica gel fertilizer Silicic acid in fertilizer was extracted with hydrochloric acid 1 23 and sodium hydroxide solution 20 g L successively and then each extract was mixed The silicic aci
242. Standard deviation of sample to sample 7 Standard devitation of sample to sample include repeatability Sbr V Sbb Sr 8 Relative standard deviation of sample to sample include repeatability 9 F value calculated based on analysis of variance ANOVA 10 F critical value F 9 10 0 05 3 02 11 Test by transmitted light analysis 12 Test by X ray diffractometric analysis 32 Vol 7 2014 3 1 2 X10 Table 1 FIED F 9 10 0 05 Te 2 Table 2 TUPAC AOAC
243. as Y j m VE ES p SR Sw COM 9 99 HbO 0 0 9 1 43 0 14 0 216 0 072 0 0 10 14 84 0 07 0 163 0 128 T N 1 0 9 14 84 0 08 0 144 0 087 2 0 8 14 83 0 09 0 140 0 062 A N 0 0 9 10 36 0 13 0 207 0 072 C PzO5 0 0 10 10 79 0 03 0 086 0 077 W K2O 0 0 10 13 07 0 08 0 158 0 096 NEN 0 0 10 1 0 i cet C M20 3 18 0 07 0 117 0 048 1 0 9 3 18 0 08 0 121 0 040 C MnO 0 0 10 0 356 0 009 0 0176 0 0123 C BzO 0 0 10 0 203 0 005 0 0094 0 0045 1 Cochran 3 2 Grubbs 4 3 sw ss RSD HorRat HorRats 5 RSDr HorRats RSDwPRSD
244. z ZIl 2 77 100 96 lzl 3 0 14 Mean Median 7 W K20 T Cd AL T 92 Vol 7 2014 ICP
245. 0 71 2009 85 39 03 0 92 24 1 47 0 62 2010 85 49 26 0 80 1 6 1 14 0 70 2011 76 49 48 0 68 14 0 97 0 70 2012 Tl 49 95 0 71 14 1 00 0 71 2013 78 36 79 0 95 2 6 1 56 0 61 C MgO 2006 78 6 18 0 13 2 0 0 67 0 19 2007 86 3 17 0 21 6 6 1 95 0 11 2008 89 5 80 0 14 24 0 79 0 18 2009 87 2 34 0 20 8 7 2 48 0 08 2010 88 5 42 0 11 21 0 67 0 17 2011 78 3 36 0 23 6 8 2 05 0 11 2012 81 6 77 0 19 2 8 0 94 0 20 2013 79 371 0 14 3 6 1 11 0 12 1 4 HorRat 2 5 Horwitz 6 2013 79 6 Median NIQR RSD HorRat HSD PS omga a o mg kg mg kg 96 mg kg Mois 136 2 93 0 84 28 7 8 42 0 10 A N 130 9 92 0 75 7 5 2 66 0 28 C P205
246. 021 significance Exchangeable Cd 0 037 0 038 0 039 0 037 0 038 significance pH EO 6 8 6 7 EC mS m 19 4 19 6 lt Standard plot SP gt 0 1 mol L HCI Cd mg kg 0 16 0 16 018 0 18 0 17 Exchangeable Cd 0 030 0 031 0 036 0 032 0 032 pH EO 6 5 6 5 Ec mS m 17 5 18 7 1 Content of cadmium dissolved with 0 1 mol L hydrochloric acid in the drying soil 2 Content of cadmium dissolved with pH 7 0 1 mol L ammonium acetate solution in the drying soil 3 Soil pH determined on 1 5 soil water suspensions with a glass electrode n 2 4 Soil electrical conductivity determined on 1 5 soil water suspensions with an electrical conductivity meter n 2 5 It is significantly different for standard plot t test 5 of both sides levels of significance n 4 2x2 repetition x number of samples 2 2013 2013 7 17 2013 10 22 A 1 3 c ii
247. 1 0 7 ARU 0 3 2 8 HorRat 0 14 1 39 HorRat 2 Table 3 Statistical analysis of collaborative study results Analysis as sulfur No of labs Mean Mean ao RSD sR RSDr Sample 1 9 9 9 f 9 HorRat p 4 a 8 2 8 32 3 33 0 02 0 7 0 05 1 4 0 42 b 10 0 12 71 5 09 0 03 0 6 0 14 2 8 0 91 c 9 1 247 6 9917 0 24 0 2 1 39 1 4 1 39 d 8 2 2456 9837 0 18 0 2 0 30 0 3 0 30 e 8 2 1 41 0 564 0 002 0 4 0 003 0 6 0 14 f 9 1 2 89 1 16 0 001 0 1 0 01 0 9 0 22 1 Number of laboratories where p number of laboratories retained after outlier removed and q number of outliers 2 Grand mean value as sulfur trioxide n The number of participating testing laboratoried p X The number of times of repetition 2 3 Grand mean value as sulfur 72 4969x Grand mean value as sulfur trioxide 4 Standard deviation of repeatability 5 Relative standard deviation of repeatability 6 Standard deviation of reproducibility 7 Relative standard deviation of reproducibility
248. 1 1 0 1 1 4 4 1 3 ERA A B OADM 2 A FE Aap 2012 11 30 2015 6 YE B I 3 ee 3 4 4 ERM Application Note 1 TES TEM FA ERM Application Note 11 COREA 1 FOU EL CR alk A B Umeas RO uy EDS Uca DES H Hy fee k REY An
249. 1 mL lt Methanol 99 mL 30 min Centrifugal separation Refining 1 Oasis HLB column Prewash the coluumn in order of methanol 5 mL and water 5 mL Centrifuge tube 50 mL 3 000 rpm 5 min lt Sample solution 5 mL Wash 2 times with sodium hydroxide 0 4 g L methanol 1 1 5 mL lt Hydrochloric acid 1 11 3 mL Refining 2 Oasis HLB column lt Prewash the coluumn in order of acetonitrile 5 mL and hydrochloric acid 1 120 5 mL Remove methanol lt Apply concentrated sample solution lt Wash 2 times with hydrochloric acid 1 120 5 mL with washed the container beforehand lt Wash with hydrochloric acid 1 120 acetonitrile 9 1 5 mL Water 5 mL Eluate with ammonia solution 0 0025 w v acetonitrile 9 1 4 mL Formic acid 1 1 000 Measuring fik 5 mL Ultracentrifugal separation LC MS MS 10 000 rpm 5 min Scheme 1 Analytical procedure for Clopyralid Aminopyralid and Picloram in fertilizers 3 1 9 CHESS m z 192 M H GE m z 207 IM H m z 241 M H 2358
250. 100g dry soil 2009 5 8 6 1 7 7 6 9 2012 4 9 5 1 6 2 6 0 CEC c molc kg 2012 35 8 36 3 36 9 37 3 0 1 mol L HCLCd mg kg 2009 0 18 0 19 0 18 0 21 2012 0 18 0 19 0 14 0 15 Kind of soil Andosol Andosol Soil texture Light clay Light clay 1 Sludge fertilizer application plot 2 Standard plot 3 Soil pH determined on 1 5 soil water suspensions with a glass electrode n 1 4 Soil electrical conductivity determined on 1 5 soil water suspensions with an electricalconductivity meter n 1 5 Content in the dry matter average n 2 6 Mass fraction 7 The year when the study was designed to evaluate the effects of sludge fertilizer aplications on soil intended for long term use 8 The year when this study was conducted ARS DD FEE OV AUD RIZE VENER OO RES ERB 45 Table 2 Properties of sludge fertilizer Properties Unit Content Property Unit Content Total nitrogen D 3 3 Total copper mg kg 546 Total phosphorus 52 Total zinc mg kg 1 760 Total potassium o D 0 4 Carbon to nitrogen ratio 7 1 Total calcium P 2 1 Total cadmium mg kg 3 6 Organic carbon o D 23 6 Acid solubility cadmium mg kg 3 2 Moisture 261 Exchangeable cadmium mg kg 0 32 1 Mass fraction 2 Content as P205 3 Content as K2O 4 Content as CaO 5 Cont
251. 17 0 18 0 34 2 Quantity of cadmium uptake Harvest dry weight x Cadmium concentration dry matter 3 It is no significantly different for standard plot t test 5 of both sides levels of significance the harvest is n 2 cadmium concentration is n 4 2x2 repetition x number of samples 4 It is significantly different for Standard plot t test 5 of both sides levels of significance the cadmium concentration and cadmium quantity of cadmium uptake are n 4 2x2 repetition x number of samples 2 0 1 mol L HCI Cd 1 mol L pH 7 0 Cd pH EC Table 10 0 1 mol L HCI Cd T Lu 0 20 mg kg w 0 05 1 mol L HE pH 7 0 Cd 0 05 0 16 mg kg T XX 0 038 mg kg 0 031 mg kg H 53 Table 10 Characteristics of soil used in this study Unit Test plot 1 Test plot 2
252. 2 13 3 S 3 4 BEPUL 5 ICP 1 5 7 4 ICP 2 1 5 np
253. 2013 HPLC 21 Determination of Melamine and Its Related Substances in Fertilizer by High Performance Liquid Chromatography HPLC A Collaborative Study Etsuko BANDO and Sigehiro KAT Food and Agricultural Materials Inspection Center Sapporo Regional Center A collaborative study was conducted to evaluate high performance liquid chromatography HPLC for determination of melamine and its related substances in fertilizers The melamine and its related substances were extracted with hydrochloric acid water 12 15 The extract was centrifuged and a portion of the supernatant was diluted with mobile phase The melamine and its related substances were analyzed by HPLC on carbamoyl modified silica gel column with UV detection at 214 nm Eleven collaborators were sent 5 sample materials in a blind duplicate design After identification of outliers with Cochran s test and Grubbs test the mean values and the reproducibility relative standard deviation RSDs of determination of melamine were reported 0 0343 2 83 and 4 2 11 6 respectively Those of determination of ammeline were reported 0 0346 1 60 96 and 2 3 6 9 96 respectively Those of determination of ammelide were reported 0 188 1 10 and 6 5 7 6 95 respectively Th
254. 55 2010 61 3 62 0 36 9 8 0 75 0 48 2011 52 4 74 0 61 12 9 1 02 0 60 2013 52 10 31 0 99 9 6 0 85 1 16 T Cd 2006 95 1 26 0 11 9 1 0 59 0 19 2007 85 124 0 12 9 6 0 62 0 19 2008 86 2 60 0 15 59 0 43 0 36 2009 73 0 47 0 08 173 0 97 0 08 2010 79 1 22 0 08 6 7 0 43 0 19 2011 74 2 03 0 09 44 0 31 0 29 2013 65 3 02 0 24 81 0 60 0 41 1 4 HorRat 2 5 Horwitz 3 6 T As T Cd mg kg 78 Vol 7 2014 5 2 2006 2013 el 2 m ete 5 a zn one p pu i SM ae S SiO gt 2006 66 33 92 0 60 1 8 1 08 0 58 2007 67 2825 0 87 3 1 1 63 0 53 2008 68 33 35 0 49 1 5 0 85 0 58 2009 69 32 67 0 62 1 9 1 09 0 57 2010 67 33 52 0 57 1 7 0 98 0 58 2011 59 30 69 0 75 2 4 1 35 0 55 2012 67 36 15 0 48 13 0 80 0 60 2013 60 35 18 0 55 1 6 0 92 0 59 AL 2006 75 50 56 0 64 13 0 91 0 71 2007 83 48 70 0 76 1 6 1 08 0 70 2008 86 50 90 071 14 0 99
255. 6 96 and 1 1 10 7 96 respectively On the basis of 7 replicate measurements of spiked samples the LOQ values were about 10 g kg as agricultural chemicals in the compost or the fertilizer Those results indicated that the developed method was valid for the determination of these agricultural chemicals Key words clopyralid aminopyralid picloram compost composted sludge fertilizer liquid chromatography tandem mass spectrometry LC MS MS Research Report of Fertilizer 7 1 9 2014 10 Vol 7 2014 2 HPLC 2 1 2
256. 8 lt P 94 12 13 25 1 4 P205 95 4 4 p 24 9 38 1 PzOs 2 DA P ELTERE RIN 6 X 9 149 96 82 53 67 43 p 33 21 47 30 96 10 zZ gt 3 5 7 8 14 ML
257. 97 0 15 0 6 0 11 0 18 0 7 1 97 Phosphate fertilizer mixture 2 10 0 34 42 0 26 0 7 0 18 0 31 0 9 2 02 Compound fertilizer 1 10 0 29 80 0 17 0 6 0 0 17 0 6 0 84 Compound fertilizer 2 10 0 33 26 0 31 0 9 0 0 31 0 9 0 85 Compound fertilizer 3 10 0 15 44 0 12 0 8 0 11 0 16 1 0 2 68 1 The number of samples used for analysis The number of outliers 2 Grand mean value n The number of samples used for analysis X The number of repetition 2 3 Mass fraction 4 Standard deviation of repeatability 5 Relative standard deviation of repeatability 6 Standard deviation of sample to sample 7 Standard devitation of sample to sample include repeatability Spar V Spp Sr 8 Relative standard deviation of sample to sample include repeatability 9 F value calculated based on analysis of variance ANOVA 10 F critical value F 9 10 0 05 3 02 2 Table 2 Cochran Grubbs 1 2 8 Table 2 Individual result of for soluble silicic acid mass Lab Phosphate Pho
258. Carrot 0 40 0 04 0 37 0 02 1 6 0 1 1 1 0 1 2012 Winter Spinach 0 35 0 02 0 33 0 03 1 7 0 1 1 3 0 1 2013 Summer Carrot 0 33 0 02 0 31 0 01 1 9 0 2 1 2 0 1 1 Content of copper and zinc dissolved with pH 7 0 1 mol L ammonium acetate solution in the drying soil 2 Sludge fertilizer applic ation plot 3 Standard plot 4 Standard deviation n 4 2 X2 repetition X number of samples 6 Table 15 Fig 6 3 4 bo 2 2009 2013 Codex 1 4 LAL 2010 Codex 0 2 mg kg 8
259. Now Kobe Regional Center Food and Agricultural Materials Inspection Center Fertilizer and Feed Inspection Department Now Sendai Regional Center This research is monitoring the change of the cadmium which was dissolved with 0 1 mol L hydrochloric acid acid solubility Cd and pH 7 0 1 mol L ammonium acetate solution exchangeable Cd from the soil We have investigated the cadmium absorption by the crop since 2009 Test field is the upland fields derived from Andosol and the used fertilizer is sludge fertilizer and chemical fertilizer We cultivated the carrot in summer 2013 and the spinach in winter 2012 Those crops were cultivated in the standard plot SP and the sludge fertilizer application plot AP The SP was used reagents and fused magnesium phosphate The AP was used the sludge fertilizer of 500 kg 10a fresh weight Other ingredients were used reagents and fused magnesium phosphate The amount of nitrogen phosphorus and potassium applied to each plot was designed on the basis of fertilization standard showed by Saitama prefecture Web site Total cadmium amount in the crop acid solubility Cd and exchangeable Cd in cultivated soil were measured by an inductively coupled plasma mass spectrometry ICP MS As a result acid solubility Cd and exchangeable Cd in the AP were indicated significantly highly content for the SP This result has been obtained from the 2011 winter crop spinach Although acid solubility Cd and exchange
260. SiO 2 7 8 8 11 4 30 34 84 52 57 88 6 55 38 22 16 4 43 7 62 35 35 S SiO gt 40 25 10 2 3 1 Merck Millipore Elix Advantage5 JIS K 0557 A3 2 0 1 mol L 0 2 mol L 8576 5 5 mL 11 mL 3 E 35 d 4 5 1 000 mL 30 mL JIS K JIS K 8180 on o n 4 JIS K 8121 5 HS K8101 4150 g 0 1 mol L 0 2 mol L 58 g 1 000 mL 1 6
261. Vol 7 2014 Table 3 Elution pattern from cartridge columun Agricultural Fraction volume ae Total chemical 0 4 mL 4 8mL 8 12 mL 12 16 mL 16 20 mL Clopyralid 89 0 0 0 0 89 Aminopyralid 87 0 0 0 0 87 Picloram 96 0 0 0 0 96 a Mean Value n 23 b Each Pesticide spiked at each 50 g kg in the sample 5 50 ng mL 2 4 1 3 50 ng mL 2 4 4 Table 4 Welch t 5 Table 4 Confirmation of sensitization or desentization effect action by sample solution Spiked Recovery of Recovery of Agricultural ab Sample level standard sample solution chemical ng mL Clopyralid 50 105 6 103 1
262. a result the mean recoveries ranged from 101 1 107 0 On the basis of 7 replicate measurements of each testing method of a solid sample and a liquid sample the limit of quantitative value LOQ was estimated at 0 004 and 0 0004 respectively These results indicated that these methods performance characteristics were available in establishing criteria for a determination method of iron Key words criteria approach iron atomic absorption spectrometry Testing Methods for Fertilizers Research Report of Fertilizer 7 131 137 2014 138 Vol 7 2014 12 I 2 1 E HEROS AAD ISO IEC 17025 ISO IEC 17025 2005 JIS Q 17025 2005 DD
263. in Inter laboratory Precision at ppb and sub ppb Concentrations in Relation to Fitness for Purpose Criteria in Proficiency Testing Analyst 125 385 386 2000 13 Horwitz W Albert R The Horwitz Ratio HorRat A Useful Index of Method Performance with Respect to Precision J AOAC Int 89 4 1095 1109 2006 155 14 25 5 1 127 23 8 30 A 105 2011 15 2013 7 68 94 2014 156 Vol 7 2014 Effect of Time during Extraction Operation on Measurements of Citric Acid Soluble Magnesium in Silicate Slag Fertilizer Souichi IGARASHI and Yasuharu KIMURA Food and Agricultural Materials Inspection Center Kobe Regional Center Now Fukuoka Regional Center Food and Agricultural Materials Inspection Center Kobe Regional Center We ha
264. proficiency testing compound fertilizer silicate slug fertilizer harmful element ISO IEC 17043 ISO IEC 17025 z score Research Report of Fertilizer 7 68 94 2014 2013 E FAMIC A 13 95 8 ROR FAMIC A 13 O 1 uuu 1 HH LESS HA A 1 ESRI Ad 2013 FE 3 1 ISO IEC 17025 2005 JIS Q17023 2005 FAMIC A ISO Guide 34 2009 JIS Q 0034 2012 5 Sir TTE mo Ale LII
265. sample solution The precipitation of barium sulfate was separated from the solution by filtration washed with water and ignited at 800 C The sulfur content as sulfur trioxide was calculated from the ignition weight of barium sulfate Six samples fertilizers containing sulfur and a sulfuric compound and sample which diluted sulfuric acid were sent to 10 collaborator These samples were analyzed as blind duplicates After removing the outlying date using Cochran and Grubbs outlier test mean values as sulfur trioxide were in the range of 1 41 to 247 6 mass fraction and the repeatability relative standard deviation RSD and the reproducibility relative standard deviation RSDs ranged from 0 1 to 0 7 96 0 3 to 2 8 96 respectively These results indicated that this method was validated for determination of sulfur content in the fertilizer Key words fertilizer sulfur sulfuric acid gravimetric analysis Research Report of Fertilizer 7 28 35 2014 36 Vol 7 2014 5 1 15
266. 0 14 As mg kg 2 38 0 04 2 36 0 05 0 02 0 13 Cd mg kg 5 89 0 03 6 04 0 05 0 15 0 12 Hg mg kg 0 89 0 01 0 86 0 01 0 03 0 03 Ni mg kg 45 6 0 5 45 3 0 6 0 3 1 6 Pb mg kg 24 7 0 6 26 2 0 7 1 5 1 9 1 7 x 2 2 3 4 5 6 k 2 7 4 FAMIC A FAMIC A 10 B FAMIC B 10 C FAMIC C 12 A B C ISO Guide 35 2006 JIS Q 0035 2008 A B
267. 0 23 1 5 0 32 AN 10 0 10 25 0 10 1 0 0 05 0 11 1 1 1 44 lt C Pz05 10 0 10 82 0 16 1 4 0 0 16 1 4 0 47 W KsO 10 0 12 92 0 08 0 6 0 0 08 0 6 0 78 lt C MgO 10 0 3 15 0 03 0 8 0 01 0 03 0 8 1 09 C MnO 10 0 0 354 0 00 25 0 004 0 010 27 1 32 C BzO 10 0 0 1956 0 000 1 5 0 002 0 004 1 9 2 27 1 O Cochran 2 x2 oo ND tA A 9 A 2 2 Spar V Sbb t Sr 10 F BES F 9 10 0 05 23 02 BRE 1 08 1 06 1 41 1 42 1 13 1 13 1 59 1 49 1 60 1 55 1 49 1 71 1 54 1 62 1 30 1 30 1 77 1 67 131 1 37 mommooun m 1 3 1 2 Cochran ff 4
268. 0 6 97 0 0012 6 94 0 03 0 001 0 003 W Ko0 22 0 8 80 0 0026 8 74 0 17 0 007 0 017 C T N 7 3 4 73 0 0032 4 75 0 08 0 008 0 102 T PzOs 7 3 8 55 0 0089 8 61 0 08 0 008 0 101 T KoO 7 3 0 58 0 0038 0 61 0 02 0 002 0 028 T CaO 7 3 5 95 0 0017 5 94 0 20 0 02 0 25 O C 7 3 20 34 0 0033 20 36 0 40 0 04 0 52 1 A B 28 C 14 2 3 A B x 2 C 3 x 4 5 6 7 8 Sp X to 95 n 2 9 Ibi Sp X to95n 2
269. 0 7 450 5 000 6 330 6 330 6 330 6 330 6 330 6 330 6 330 0 745 71 050 74 443 74 745 EDT A X III 75 401 3 770 0 3770 7 540 0 754 0 075 0 075 0 0075 7K 67 280 74 066 74 745 74 813 Fe 10 0 5 0 05 1 0 1 0 01 0 01 0 001 D 2 3 D MERCK ELIX ESSENTIALS JIS K 0557 A3 2 JISK8180 3 Fe 0 1 mg mL Fe 100 mg L JCSS 4 Fe 0 1 mg mL 1l 5 Fe 0 05 ug mL 6 0 ug mL Les 5 1 5 KT 4 fEUCAIRUT 4 W Fe 3 1 W Fe
270. 014 123 10 NP 1 ISO IEC 17025 2005 JIS Q 17025 2005 ISO IEC 17025 criteria Criteria Approach y dd Nd decia
271. 1 10 15 20 H 13 C 1C 116 Vol 7 2014 38 4 2 0035 2008 bi KO Fr bg f gs XX sy Tex A A 2 A B 0 7H 12 20 7 24 28 32 7 d e 4 1 KUK ISO Guide 35 2006 JIS Q LO s sp to 95 n 2
272. 1 23 30 1 g 1 mg 250 mL 1 23 1150 mL 1530 C TUE 30 40 N yA di 30 1 C 1 200 mL 10 mL 15 mL 2 g 30 6 6 7 300 mL 7k 0 1 moVL 0 2 molL 1 3 1 S SiO gt 3 2 4 0 5 126
273. 18 0 028 3 9 0 052 ED 1 72 Ammonium sulfate 11 0 0 0345 0 0031 8 9 0 0056 16 1 2 43 1 8 Refer to the footnote of Table 4 1 Table 4 4 Statistical analysis of collaborative study results for cyanuric acid No of labs Mean s RSD5 sre RSD rr 8 Sample 1 3 3 3 HorRat p q Calcium cyanamide 1 9 2 1 15 0 06 4 8 0 09 7 7 1 97 Calcium cyanamide 2 10 1 0 390 0 018 4 5 0 029 7 4 1 61 RU 9 2 0 105 000 29 0 014 13 2 235 containing Calcium cyanamide Compound fertilizer 9 2 0 788 0 026 3 2 0 054 6 8 1 65 Ammonium sulfate 10 1 0 0365 0 0015 4 2 0 0067 18 3 2 78 1 8 Refer to the footnote of Table 4 1 HPLC 19 Q05 4 paces Fig 1 HPLC chromatogram of melamine and its related substances in ammonium sulfate Substance name 1 Cyanuric acid 2 Ammelide 3 Melamine 4 Ammeline 4 11 5 10 HPLC R 0 0343 2 83
274. 2013 1 A B 2012 11 C 2 1 1 ISO Guide 35 2006 JIS Q 0035 2008 Clit t
275. 31 ISO Guide 35 collaborative study Research Report of Fertilizer 7 95 104 2014 105 nan zu 20134E BE E 9 201378 FAMIC A 10 FAMIC B 10 FAMIC C 12 ISO Guide 31 ISO Guide 35 1 FAMIC
276. 35 7 0 2 21 0 16 2008 145 2 87 0 24 8 5 2 50 0 10 2009 145 3 53 0 15 42 1 27 0 12 2010 143 1 58 0 41 26 0 6 97 0 06 2011 137 1 00 0 12 12 0 3 00 0 04 2013 136 2 93 0 84 28 7 8 42 0 10 T N 2006 158 14 60 0 13 0 9 0 33 0 38 2007 145 8 74 0 07 0 8 0 26 0 25 2010 140 14 11 0 11 0 8 0 30 0 38 A N 2006 150 11 46 0 10 0 9 0 33 0 32 2007 143 6 20 0 09 1 4 0 47 0 19 2008 147 12 56 0 16 12 0 45 0 34 2000 144 5 56 0 07 1 3 0 43 0 17 2010 128 11 53 0 18 1 6 0 56 0 32 2011 138 13 49 0 18 1 3 0 49 0 36 2012 130 2 39 0 04 1 9 0 53 0 08 2013 136 9 92 0 74 7 5 2 63 0 28 N N 2009 TY EET 123 3 62 0 11 3 2 0 96 0 12 2012 115 2 17 0 10 4 8 1 34 0 08 T POs 2007 140 10 35 0 10 0 9 0 33 0 29 C P20s 2007 143 9 81 0 13 1 3 0 47 0 28 2008 146 15 82 0 13 0 8 0 32 0 40 2010 141 14 59 0 18 1 2 0 47 0 38 2013 129 20 60 0 20 1 0 0 44 0 45 S P20s 2006
277. 383 0 383 0 853 0 831 0 203 0 198 0 0392 0 0365 C 2 85 2 85 0 396 0 395 0 877 0 860 0 199 0 195 0 0318 0 0297 D 3 05 3 02 0 440 0 435 1 10 0 962 0216 0212 0 0589 0 0472 E 2 96 2 96 0 405 0 401 0 907 0 843 0 207 0 201 0 0374 0 0384 F 2 77 2 80 0 354 0 361 0 807 0 815 0 170 0 171 0 0267 0 0285 G 2 80 2 76 0 4410 0 378 0 860 0 827 0 181 0 190 0 0373 0 0338 H 2 83 2 90 0 400 0 404 0 880 0 888 0 208 0 209 0 0365 0 0340 I 269 281 0 393 0 301 0 868 0 863 0 198 0 195 0 0348 0 0353 J 2 00 2 64 0 362 0 363 0 777 0 786 0 197 0 192 0 0336 0 0335 K 2 37 1 61 2 0 391 0 399 0 845 0 501 0 191 0 209 0 0287 0 0314 1 Laboratory identification 2 Outlier of Cochran 3 Outlier of Grubbs HPLC 15 Table 3 2 Individual result of ammeline mass Lab Calcium Calcium NG ie terhe Compound Ammonium IDD cyanamide 1 cyanamide 2 epee osu fertilizer sulfate cyanamide A 1 53 1 57 0 105 0 103 0 585 0 591 0 192 0 187 0 0381 0 0341 B 1 58 1 37 0 106 0 106 0 635 0 622 0 196 0 192 0 0378 0 0356 C 1 59 1 58 0 102 0 101 0 634 0 630 0 195 0 194 0 0311 0 0290 D 1 48 1 47 0 104 0 105 0 685 0 581 0 191 0 191 0 0457 0 0292 E 1 64 1 65 0 106 0 108 0 656 0 610 0 200 0 195 0 0368 0 0372 F 1 62 1 63 0 102 0 103 0 619 0 627 0 185 0 189 0 0320 0 0323 G 1 68 1 67 0 115 0 105 0 648 0 645 0 212 0 214 0 0345 0 0326
278. 397 0 398 0 200 0 206 20 3 30 3 41 0 388 0 388 0 208 0 210 24 3 32 3 38 0 397 0 400 0 211 0 217 28 3 33 3 36 0 412 0 420 0 213 0 218 32 3 28 3 44 0 385 0 389 0 198 0 219 38 3 4 44 3 44 0 397 0 406 0 203 0 218 3B B ul y A N S P20s W P20s W K20 0 8 33 8 49 7 99 8 03 6 88 6 94 8 59 8 75 12 8 27 8 30 8 11 8 11 7 01 7 01 8 81 8 84 20 824 8 31 8 08 8 09 6 99 7 00 8 65 8 70 24 8 17 8 18 8 00 8 17 6 96 6 98 9 02 9 04 28 8 32 8 33 8 14 8 17 6 04 6 96 8 96 9 05 32 8 21 8 22 8 16 8 17 6 904 6 98 8 60 8 68 38 8 36 8 39 8 02 8 08 7 00 7 01 8 71 8 79 3B mg kg ul 5 i As Cd Hg Ni Pb 0 2 60 2 63 5 83 5 84 0 881 0 890 42 4 45 5 23 7 23 7 12 2 32 2 48 5 93 5 95 0 885 0 889 47 3 47 3 25 8 26 9 20 2 25 2 25 5 86 5 89 0 856 0 871 44 8 45 6 24 8 26 9 24 2 38 2 39 5 99 6 01 0 891 0 892 45 1 46 5 25 7 26 3 28 227 2 32 5 87 5 99 0 933 0 945 46 8 46 9 21 5 22 9 32 2 28 2 34 5 82 5 82 0 888 0 916 43 6 44 8 24 6 25 6 38 2 34 2 42 5 76 5 85 0 868 0 873 46 1 46 1 21 6 25 9
279. 45 0 351 0 310 0 364 0 339 0 201 0 203 0 199 0 200 0 210 0 204 C 0 382 0 391 0 392 0 362 0 349 0 349 0 198 0 201 0 200 0 194 0 193 0 193 D 0 320 0 321 0 336 0 342 0 359 0 333 0 199 0 202 0 206 0 199 0 200 0 204 E 0 344 0 340 0 337 0 341 0 336 0 340 0 210 0 208 0 211 0 207 0 209 0 209 F 0 345 0 345 0 354 0 347 0 351 0 358 0 187 0 191 0 195 0 199 0 199 0 200 G 0 353 0 350 0 357 0 359 0 360 0 356 0 194 0 195 0 186 0 188 0 188 0 183 H 0 375 0 371 0 371 0 361 0 378 0 363 0 215 0 222 0 211 0 216 0 208 0 214 I 0 345 0 364 0 361 0 381 0 369 0 370 0 201 0 199 0 201 0 212 0 209 0 217 J 0 366 0 358 0 371 0 346 0 365 0 359 0 191 0 193 0 202 0 199 0 190 0 201 1 2 Cochran 3 1 4 100 Vol 7 2014 4 A a 2 A SEA EE ZS 1 2 yx
280. 5 g 1 mol L pH 7 0 50 mL 20 30 C 1 ICP 48 Vol 7 2014 2 2013 2013 7 17 2013 10 22 A 1 2 1 ETE pH EC 19 0 1 mol L HCI Cd Table 5 Table 5 Characteristics of soil used in this study Unit year AP 1 AP 2 spP2 1 SP pH HO 2009 6 1 6 1 6 2 6 2 20139 6 8 6 7 6 5 6 5 EC mS m 2009 10 0 10 3 14 0 11 6 2013 19 4 19 6 17 5 18 7 Total nitrogen 9 2013 0 42 0 43 0 40 0 42 Total carbon gt 9 2013 5 6 5 6 5 4 5 5 Available phosphate 5 mg 100g dry soil 2009 5 8 6 1 7 7 6 9 2013 5 4 5 4 8 2 7 3 0 1 mol L HCLCd mg kg 2009 0 18 0 19 0 18 0 21 2013 0 20 0 21 0 16 0 18 Kind of soil Andosol Andosol Soil texture Light clay Light clay 1 Sludge fertilizer application plot 2 Standard plot 3 Soil pH dete
281. 8 Horwitz ratio of reproducibility 9 Mass fraction 4 10 6 12 0 3 2 8 ux 34 Vol 7 2014 Lu D
282. 8 10 75 10 80 10 85 10 87 10 75 D 10 56 10 46 10 57 10 37 10 36 10 38 10 97 10 87 10 94 10 75 10 68 10 71 E 10 07 10 07 9 99 10 05 10 04 10 06 10 77 10 83 10 92 10 82 10 88 10 73 F 10 18 10 28 10 19 10 38 10 26 10 10 10 70 10 79 10 89 10 95 10 95 10 91 G 10 54 10 53 10 53 10 54 10 55 10 59 10 70 10 80 10 75 10 86 10 82 10 93 H 10 63 10 63 10 62 10 45 10 45 10 56 10 81 10 79 10 77 10 69 10 73 10 78 I 10 21 10 20 10 22 10 25 10 23 10 25 10 66 10 68 10 78 10 73 10 57 10 71 J 10 31 10 28 10 40 10 30 10 37 10 39 10 83 10 82 10 83 10 78 10 80 10 80 lt A 13 29 13 12 12 96 13 03 12 99 12 98 3 29 3 25 3 32 3 20 3 20 3 13 B 13 02 12 84 12 79 13 13 13 02 12 93 3 29 3 20 3 22 3 03 3 14 3 10 C 13 24 13 57 13 39 13 21 13 06 13 17 3 23 327 3 26 3 22 3 17 3 17 D 13 15 13 10 13 27 13 25 1327 13 31 3 11 3 11 3 15 3 11 3 17 3 09 E 12 87 12 85 12 88 12 86 12 83 12 80 3 36 3 40 3 37 3 4 3 36 3 35 F 12 89 13 03 12 91 13 02 12 98 13 04 3 16 3 15 3 12 3 21 3 19 3 18 G 13 19 13 14 13 19 13 08 13 04 13 06 3 16 3 20 3 18 3 23 325 322 H 13 24 13 13 13 14 13 16 13 19 13 17 A 3 19 3 20 3 25 3 20 3 22 3 18 I 13 07 13 09 13 05 12 84 12 91 12 98 2 96 2 90 3 00 2 94 2 91 2 92 J 13 12 13 11 13 07 13 07 13 06 13 13 3 13 323 3 16 3 10 3 16 3 19 A 0 383 0 365 0 395 0 352 0 367 0 358 0 210 0 215 0 218 0 213 0 212 0 217 B 0 342 0 3
283. 8 7 2013 FED HorRat 1 11 NIQR 0 14 96 Horwitz F HSD 0 12 2013 C MgO Median 3 77 2007 2011 Median 2 34 3 36 154 Vol 7 2014 4 C MgO RSD 6 8 8 7 RSDr 2 1 2 8
284. 9 18 9 26 14 90 15 11 21 05 19 87 35 84 35 94 38 81 38 91 B 996 953 15 72 16 00 22 00 20 63 34 57 35 04 37 74 317 68 C 9 07 8 88 14 68 14 89 20 05 21 45 34 00 34 3 37 72 37 22 D 9 63 9 69 14 81 14 65 20 19 20 63 34 92 34 96 38 13 37 69 E 9 25 9 19 15 12 15 28 20 66 20 29 35 19 35 19 39 26 39 06 F 8 96 8 99 14 78 14 30 18 39 19 27 33 87 34 09 37 42 36 93 G 10 07 9 84 14 96 14 73 20 88 18 93 34 86 34 94 37 9 38 54 H 9 63 9 81 15 33 15 79 21 67 20 45 34 97 35 01 38 33 38 18 I 9 37 9 80 14 90 15 28 21 02 20 64 35 53 35 55 38 82 39 25 1 Laboratory identification 2 Invalid datas that were removed due to failure of the operation 3 Outlier of Cochran Table 4 Statistical analysis of collaborative study results 2 4 6 Sons No of cn cd Sr A RSD SR 2 RSDr HorRat p q Calcined sludge fertilizer 9 0 9 45 0 17 1 8 0 38 4 0 1 40 Industrial sludge fertilizer 8 1 15 13 0 20 1 3 0 42 2 8 1 09 Compost 9 0 20 50 0 76 3 7 0 94 4 6 2 08 Human waste sludge fertilizer 8 1 34 96 0 07 0 2 0 62 1 8 1 05 Composted sludge fertilizer 9 0 38 20 0 27 0 7 0 73 1 9 1 18 1 Number of laboratories where p number of laboratories retained after outlier removed and q number of outliers 2 Grand mean value n The number of participating testing laboratories p X The number of repetition 2 3 Mass fraction 4 Standard deviation of repeatability 5 Relative standard deviation of repeatability 6 S
285. 92 FE 129 5 25 6 2006 20 6 E3 16 H t 59 4 704 1999 7 25 1 605 1 198 18 3 23 E 11 4E 5 H 13 127 7 23 4 E8 30 51 105 2011 8 AOAC Guidelines for Single Laboratory Validation of Chemical Methods for Dietary Supplements and Botanicals AOAC INTERNATIONAL 2002 9 Codex Guideline on Analytical Terminology CAC GL 72 2009 2009 Fee PRK BES ER i IESE ESE CIES PIE BED ZA XE BU de XE 60 25 EO 4 284 26 9 1 25 4 H 47 2014 10 11 4 1
286. A 13 97 2013 2 3 1 Cochran ier
287. E E C oe H C BzOs 48 4 20 mg mL 1 4 5 1 IUPAC T 6 AR 4 3 3 10 2 mo 3 E 3 A 320 10 2 FAMIC
288. Fertilizers Conducted in Fiscal Year 2013 Aiko YANO Masaki CHIDA Etsuko BANDO Chika SUZUKI Yasushi MIY ASHITA Shigeyuki INAB A Natsuki TOYODOMES Yuji SHIRAI and Masashi UWASAWA Food and Agricultural Materials Inspection Center Fertilizer and Feed Inspection Department Now Fukuoka Regional Center Food and Agricultural Materials Inspection Center Sapporo Regional Center 3 Food and Agricultural Materials Inspection Center Sendai Regional Center Food and Agricultural Materials Inspection Center Nagoya Regional Center Now Ministry of Agriculture Forestry and Fisheries Tokai Regional Agricultural Administration Office Food Safety and Consumer Division Food and Agricultural Materials Inspection Center Kobe Regional Center Food and Agricultural Materials Inspection Center Fukuoka Regional Center 7 Food and Agricultural Materials Inspection Center Fertilizer and Feed Inspection Department 8 Japan Fertilizer and Feed Inspection Association A proficiency testing of analytical laboratories was conducted in fiscal year 2013 using reference materials of ground compound fertilizer and silicate slag fertilizer based on ISO IEC 17043 Conformity assessment General requirements for proficiency testing Moisture Mois ammonium nitrogen A N citric acid soluble phosphorus C P20s water soluble phosphorus W P2Os water soluble potassium W K20 citric acid soluble magnesium C MgO water soluble magne
289. H 1 61 1 65 0 104 0 107 0 629 0 635 0 197 0 199 0 0345 0 0330 I 1 57 1 63 0 108 0 108 0 641 0 631 0 199 0 199 0 0360 0 0365 J 1 62 1 63 0 107 0 106 0 598 0 601 0 204 0 193 0 0355 0 0350 K 1 24 0 917 0 110 0 106 0 557 0 307 0 175 0 187 0 0345 0 0354 1 Laboratory identification 2 Outlier of Cochran 3 Outlier of Grubbs Table 3 3 Individual result of ammelide mass 96 Lab Calcium Calcium OP ue oe Compound Ammonium ID cyanamide 1 cyanamide 2 PE on fertilizer sulfate cyanamide A 1 02 1 10 0 364 0 359 0 185 0 183 0 660 0 699 0 0388 0 0382 B 1 21 0 929 0 367 0 357 0 193 0 185 0 695 0 716 0 0424 0 0348 C 1 13 1 11 0 368 0 365 0 198 0 195 0 747 0 700 0 0284 0 0302 D 1 19 1 17 0 411 0 404 0 246 0 214 0 790 0 782 0 0460 0 0437 E 1 15 1 14 0 373 0 377 0 207 0 192 0 772 0 777 0 0377 0 0356 F 1 21 1 23 0 357 0 368 0 202 0 205 0 745 0 721 0 0299 0 0372 G 0 988 1 01 0 353 0 327 0 163 0 165 0 716 0 749 0 0358 0 0306 H 1 13 1 16 0 331 0 349 0 187 0 189 0 784 0 718 0 0337 0 0290 I 1 06 1 08 0 373 0 374 0 201 0 200 0 747 0 705 0 0330 0 0387 J 0 983 0 969 0 322 0 317 0 170 0 169 0 641 0 630 0 0313 0 0298 K 1 04 0 522 0 358 0 365 0 189 0 108 0 611 0 684 0 0266 0 0268 1 Laboratory identification 2 Outlier of Cochran
290. HED SEU n x 0 1 mol L HCI Cd Fig 7 gt 0 05 LAL E 2011 FRIEFET Table 16 Fig 7 2011 5 gt 0 05 1 5 5 DHE 1 UR ave 36 g ha emai 0 1 mol L HCI Cd 91 1 g ha pH 6 0 6 7 HEO 0 1 mol L HCI Cd 0 15 mg kg
291. HorRat G AOAC 9 0 5 lt HorRat 2 HorRatr NIQR HSD i HorRat H i mEn TH RM C Ee S 5 1 2 8 X 10 2 F 5 RSD RSD
292. MS Hisanori ARAYA Toshiharu YAGI Yoshimi HASHIMOTO and Yuji SHIRAI Food and Agricultural Materials Inspection Center Fertilizer and Feed Inspection Department Now Ministry of Agriculture Forestry and Fisheries Food Safety and Consumer Affairs Bureau Food and Agricultural Materials Inspection Center Fertilizer and Feed Inspection Department An analytical method for simultaneous determination of agricultural chemicals clopyralid aminopyralid and picloram in cattle manure compost and composted sludge fertilizer containing pig or cattle manure by liquid chromatography electrospray ionization tandem mass spectrometry LC ESI MS MS was developed The agricultural chemicals were extracted with methanol under alkaline condition The extract were purified two times with copolymer cartridge columns on different pH conditions and analyzed by LC ESI MS MS The LC separation was carried out on a C18 column using solvent gradient with formic acid solution 1 1 000 and methanol as a mobile phase The determination was performed in selected reaction monitoring SRM mode As a result of 3 replicate analysis of 5 fertilizer samples 2 kinds of cattle manure compost 2 kinds of compost sludge fertilizer containing cattle manure and 1 kind of compost sludge fertilizer containing pig or cattle manure spiked with each agricultural chemical at 40 400 and 1000 ug kg the mean recoveries and the relative standard deviations RSD were 71 2 117
293. Mo 0 002 0 0006 0 0003 3 W Mo R 0 210 NIQR 0 010 4 7 ux 1 3 W Mo W Mo
294. NIQR RSD Hoa HSD aK ES RREK o W 95 2007 86 3 17 0 21 6 6 1 95 0 11 2009 87 2 34 0 20 8 7 2 48 0 08 2011 78 3 36 0 23 6 8 2 05 0 11 2013 79 3 77 0 14 3 6 1 11 0 12 1 2 3 4 HorRat 5 Horwitz ERN 6 8 2013 2013 2007 EEE 2013 C MgO 1 3 2013 C MgO RSD 3 6 2007 2011 FED RSD 6 6
295. NTEC THM062FA ao 132 Vol 7 2014 1 JIS K8960 HS K9016 DAP JIS K8121 JIS K8617 EDTA IIT 2 x ee sei a Fe 10 Fe 0 5 Fe 0 05 Fe 1 Fe 0 1 Fe 0 01 Fe 0 01 Fe 0 001 11 400 11 400 11 400 11 400 11 400 11 400 11 400 11 400 7 450 7 450 7 450 7 450 7 450 7 450 7 45
296. able Cd content in the SP soil from 2009 summer to 2013 summer showed significantly decreasing trend in the SP the Cd content in the AP soil did not show significantly increasing or decreasing trend in the AP by the continuous application of sludge fertilizer Key words sludge fertilizer continuous application cadmium Research Report of Fertilizer 7 43 67 2014 68 Vol 7 2014 7 2013 gt 2 3 4 FORES 7 ISO IEC 17043 ISO IEC 17025 z 1 ISO IEC 17025 JIS Q 17025
297. and compost Key words organic carbon sludge fertilizer compost combustion method collaborative study Research Report of Fertilizer 7 22 27 2014 28 Vol 7 2014 4 1 SO JIS 249 S 1
298. ang DONG Fengshou XU Jun LU Caihong Simultaneous Determination of Aminopyralid Clopyralid and Picloram Residues in Vegetables and Fruits Using Ultra Performance Liquid Chromatography Tandem Mass Spectrometry AOAC Int 95 554 559 2012 4 f LC MS MS 16 17 29 2008 5 LC MS MS 3 51 59 2010 6 FAMIC lt http www famic go jp ffis fert sub9 html gt zm LC MS MS 9 Determination of Clopyralid Aminopyralid and Picloram in Compost and Composted Sludge Fertilizer by Liquid Chromatography Tandem Mass Spectrometry LC MS
299. borative Study lt Investigation and Research gt 6 Effect of Continuous Application of Sludge Fertilizer on Cadmium Absorption of the Crop and Accumulation of Cadmium in the Soil Continued Report chee ars Toshiaki HIROI Souichi IGARASHI Masahiro ECHI Yoshimi HASHIMOTO and Fumihiro ABE 43 lt Assurance Practices for Reliable Analytical Data gt 7 Result of Proficiency Testing for Determination of Major Components and Harmful Elements of Ground Fertilizers Conducted in Fiscal Year 2013 ne Aiko YANO Masaki CHIDA Etsuko BANDO Chika SUZUKI Yasushi MIYASHITA Shigeyuki INABA Natsuki TOYODOME Yuji SHIRAI and Masashi UWASAWA 68 8 Preparation of Certified Reference Material CRM for Determination of Major Components High Analysis Compound Fertilizer FAMIC A 13 Shinichi KASHIMA Toshiharu YAGI Hisanori ARAYA Satono AKIMOTO Mariko FUJITA Yoshimi HASHIMOTO Toshiaki HIROI Yuji SHIRAI and Akira KUBO Long term Stability Evaluation of Fertilizer Certified Reference Materials for Determination of Major Components and Harmful Elements High Analysis Compound Fertilizer FAMIC A 10 Ordinary Compound Fertilizer FAMIC B 10 and Composted Sludge Fertilizer FAMIC C 12 OL Shigeyuki INABA Yasuharu KIMURA Taku FUJITA Keisuke AOYAMA Kouhei ITOU Masanori HASEGAWA and Yuji SHIRAI lt Note gt 10 Verification of Performance Characteristics of Testing Method for Soluble Silic
300. cle size Guard column TOSOH corporation TSKgel guardgel Amide 80 3 2 mmx15 mm Column temperatures 40 C 1 C Mobile phase Acetonitrile phosphate buffer 4 1 Flow rate 1 0 mL min Detector system UV detector at a wavelangth of 214 nm 4 IUPAC ISO AOAC 10 2 3 5 11 10 3 Waters 2695 Series Prominence Series z Vol 7 2014 Prominence Series LC 30A LC 20A Series
301. d examined the reason that reproducibility of citric acid soluble magnesium C MgO using silicate slag fertilizer sample about proficiency testing of analytical laboratories was poor That problem was suggested a difference in manufacturing process of silicate slag fertilizer sample The manufacturing process could divide into air cooling and water cooling blast furnace slags The dissolution rate of citric acid soluble magnesium C MgO using water cooling slag was faster than air cooling one Moreover citric acid soluble magnesium C MgO using air cooling slag dissolved insidiously over set time of extraction written Testing Methods for Fertilizers Thereby in case of the analysis citric acid soluble magnesium C MgO using air cooling slag it is necessary immediate cool handling after extraction We obtained a result of difference of the dissolution rate of citric acid soluble magnesium C MgO in extraction temperature As a result in order to analyze accurately citric acid soluble magnesium C MgO using air cooling slags it is important keeping strictly to set extraction temperature writtern Testing Methods for Fertilizers and necessary immediate cool handling after extraction Key words silicate slag fertilizer citric acid soluble magnesium C MgO Testing Methods for Fertilizers Research Report of Fertilizer 7 145 156 2014 Hi
302. d in the mixture was determined by potassium fluoride method Five samples of fertilizers containing silica gel fertilizer respectively were sent to 8 collaborators These samples were analyzed as blind duplicates Mean values reported from 15 76 to 34 50 the relative standard deviation RSD for repeatability ranged from 0 4 96 to 0 7 96 the relative standard deviation RSDg for reproducibility ranged from 1 3 to 2 0 96 These results indicated that this method has an acceptable precision for determination of soluble silicic acid in fertilizers containing silica gel fertilizer Key words soluble silicic acid potassium fluoride method silica gel fertilizer collaborative study Research Report of Fertilizer 7 36 42 2014 H 43 6 eH PABA BR IER 4 ae 1 IN I Lu 0 0005
303. els of significance n 4 2x2 repetition x number of samples 8 It show that regression is significant in p 0 05 5 of both sides levels of significance 4 1 mol L WE pH 7 0 Cd 1 mol L pH 7 0 Cd 2009 2013 Table 13 Fig 4 1 mol L PEZ PH 7 0 Cd 2010 6 1 mol L HE pH 7 0 Cd p 96 Table 13 2013 gt 0 0 2012 lt 0 05 0 1 mol L HCI Cd Table 12 Fig 3 H
304. ent of cadmium dissolved with 0 1 mol L hydrochloric acid 6 Content of cadmium dissolved with pH 7 0 1 mol L ammonium acetate solution Table 3 Properties of the reagent Property Unit Ammonium Ammonium Potassium sulfate dihydrogenphosphate chloride Total nitrogen o P 21 1 12 0 Total phosphorus 9p 61 5 Total potassium 9 63 1 1 Mass fraction 2 Content as P205 3 Content as K O 3 1 4 m IE 2 mx FE m L 2 4 Fig 1 1 2 10a 30 Ae Lic f 6 2 mg 100g PERO AHE 1 Li
305. es Waters 2695 Series Table 2 1 2 4 YC F F 9 10 0 05 Table 2 1 Homogeneity test results of melamine No of Sample 1 sample Calcium cyanamide 1 10 0 Calcium cyanamide 2 10 0 Compound fertilizer containing 10 0 Calcium cyanamide Compound fertilizer 10 0 Ammonium sulfate 10 0 2 Mean 2 96 2 16 0 378 0 852 0 186 0 0366 4 Sr 96 0 02 0 005 0 022 0 002 0 0012 RSD 0 8 1 3 2 6 1 3 3 3 1 The number of samples used for analysis The number of outliers 6 Sbb 9 0 02 0 003 0 022 7 Sb r 96 0 03 0 005 0 031 0 002 0 0012 2 Grand mean value n The number of samples used for analysis X The number of repetition times 2 3 Mass fraction 4 Standard deviation of repeatability 5 Relative standard deviation of repeatability 6 Standard deviation of sample to sample 7 Standard devitation of sample to sample include repeatability Spar V Spp Sr 8 Relative standard deviation of sample to sample include repeatability 9 F value calculated based on analysis of variance ANOVA 10 F critical value F 9 10 0 05 23 02
306. etermined volume Room temperature Type 3 filter paper Transfer the same volume of sample solution 1 and sample solution 2 to 200 mL beaker made of polyethylene lt About 10 mL of hydrochloric acid lt About 15 mL of potassium fluoride solution lt About 2 g of potassium chloride Standing to cool For 30 minutes in a refrigerator Gooch crucible made of polyethylene Type 6 filter paper Wash 6 7 times with potassium chloride solution Transfer Water until the liquid volume reaches about 200 mL 70 C 80 C 300 mL tall beaker water lt A few drops of phenolphthalein solution 1 g 100 mL Scheme 1 Flow sheet for soluble silicic acid in fertilizers containing silica gel fertilizer 0 1 mol L 0 2 mol L sodium hydroxide solution Until the solution becomes light red 38 Vol 7 2014 3 1 00 g 300 mL 30 1 23 150 mL 30 C2 10 60 250 mL 6
307. f testing methods for the several form of manganese was assured from 3 replicate determinations of 2 fertilizer samples containing 0 1 96 2 5 water soluble molybdenum which were prepared each test As a result the mean recoveries ranged from 100 2 100 8 On the basis of 7 replicate measurements of each testing method of a solid sample and a liquid sample the limit of quantitative value LOQ was estimated at 0 006 and 0 0006 respectively Reported in Research Report of Fertilizer medians normalize interquartile ranges NIQR and relative standard deviations RSDr for reproducibility of water soluble molybdenum obtained by proficiency testings were 0 210 96 0 010 and 4 7 respectively These results indicated that these methods performance characteristics were available in establishing criteria for a determination method of water soluble molybdenum Key words criteria approach molybdenum sodium thiocyanate absorptiometric analysis Testing Methods for Fertilizers Research Report of Fertilizer 7 138 144 2014 E 145 13 lt
308. ic Acid in Fertilizer 11 12 13 by Potassium Fluoride Method Verification of Performance Characteristics of Testing Method for Iron in Fertilizer by Atomic Absorption Spectrometry Verification of Performance Characteristics of Testing Method for Water soluble Molybdenum Content in Fertilizer by Sodium Thiocyante Absorptiometric Analysis ELLE Keiji YAGI Natuki TOYODOME Tokiya SUZUKI and Hideo SOETA Effect of Time during Extraction Operation on Measurements of Citric Acid Soluble Magnesium in Silicate Slag Fertilizer 95 105 123 131 138 145 LC MS MS 1 LC MS MS 7 AHAA S 1 Fix
309. ics of a Method of Analysis AOAC INTERNATIONAL 2005 7 25 5 1 127 23 8 30 H 105 2011 8 25 6 20 H 64 26 9 1 47 2014 9 59 3 16 700 26 9 1 1148 2014 10 12 8 31 A 1163 26 9 1 A 1151 2014 27 Determination of Organic Carbon in Sludge Fertilizer and Compost by Hyd
310. im jp E3 P jp E3 P 11 0 y 0 0028x 10 12 10 5 9 5 0 10 20 30 40 3 A 4 A y 3E 06x 0 399 S lt R K imi ky Ss 0 10 20 30 40 0 10 20 30 40 5 A 6 A lt 0 24 S St 0 22 2o SOS gi 0 20 iy BL 0 10 20 30 40 7 A X 1A 112 Vol 7 2014 9 0 i y 0 002x 8 34 y 0 0022x 8 05 yr Ei P 0 10 20 30 40 0 10 20 30 40 H Lili TEER 2 B
311. ium Concentration Season Test crops accumu of cadmium accumu of cadmium load removal gt load removal A lation accumulation lation accumulation mg plot mg plot mg plot mg kg mg plot mg plot mg plot mg kg Summer Carrot 4 84 0 54 4 30 0 011 0 0 50 0 50 0 001 Winter Spinach 4 40 1 18 3 22 0 008 0 1 34 1 34 0 003 Summer Spinach 3 30 0 72 2 58 0 006 0 0 96 0 96 0 002 Winter Qinggengcai 2 64 0 21 2 43 0 006 0 0 21 0 21 0 001 Summer Turnip 3 30 0 15 3 15 0 008 0 0 16 0 16 0 000 Winter Spinach 7 04 0 68 6 35 0 016 0 0 58 0 58 0 001 Summer Carrot 7 28 0 73 6 55 0 016 0 0 68 0 68 0 002 Winter Spinach 7 28 0 75 6 53 0 016 0 0 75 0 75 0 002 Summer Carrot 7 28 0 46 6 82 0 017 0 0 34 0 34 0 001 Total 47 36 5 42 41 93 0 105 0 00 5 53 5 53 0 014 1 It show every test plot the quantity of cadmium load 025 mum the quantity of cadmium accumulation 10 E the 0 1 mol L HCLCd density of cultivated soil Sludge fertilizer application plot AP E 0 20 OO 8 E ws gs e 0 15 6 E E Ba 3 9 0 10 i HE 0 05 2 0 00 0 amp Carrot Spinach Spinach Qing geng cai Tumip Spinach Carrot Spinach Carrot 2 Examination Summer Winter Summer Winter Summer Winter Summer Winter Summer start 2009 2009 2009 2010 2010 2011 2011 2012 2012 2013 the crops body and quantity of cadmium accumulation to the soil Sludge fertilizer application plot AP Standard plot SP Quantity of cadmium Concentration
312. ls of significance n 4 2x2 repetition x number of samples 7 It is significantly different for Processing examination section t test 5 of both sides levels of significance n 4 2x2 repetition x number of samples 8 It show that regression is significant in p 0 05 5 of both sides levels of significance 0 05 ob E 0 04 S T T T 5 2 jJ l ji z I o i T 0 03 1 i Sludge fertilizer application plot AP d Standard plot SP Spinach Spinach Qing geng cai Turnip Spinach Carrot Spinach Carrot After winter After summer After winter After summer After winter After summer After winter After summer cultivation cultivation cultivation cultivation cultivation cultivation cultivation cultivation 2009 2010 2010 2011 2011 2012 2012 2013 Fig 4 Changes of the exchangeable Cd density of cultivated soil The error bar indicating the standard deviation 5 1 mol L ME pH 7 0 Cu Zn 1 mol L HE pH 7 0 Cu Zn 2009 2013 Table 14 Fig 5
313. mL 1 120 5 mL 2 1 120 9 1 5 mL 5 LC MS MS 3 mL 5 mL 0 0025 w v 9 1 4 mL 1 1 000 1 5 mL 10 000 rpm 8 000xg 5 Mm 4 WEkZuMZZZALCT BBWED REC LIOS RERAN OVE AMER 5 uL ILC MS MS Table 1 Table 2
314. mes transparent lt About 1 mL Hydrochloric acid 2 1 lt Water the liquid volume to reach about 100 mL Boil for 5 minutes lt About 6 mL of thermal barium chloride solution 100 g L while shaking Standing to cool For several minutes lt A few drops of thermal barium chloride solution 100 g L Check that new precipitate is no longer formed lt About 2 mL of thermal barium chloride solution 100 g L while shaking Heating 80 C 90 C 2 hours Standing to cool For no less than 4 hours in a water bath whose heat source is stopped Type 5 C fiter paper Type 5 C fiter paper water Wash with water until reaction of chloride disappears in filtrate Put Crucible Drying apparatus about 120 C 1 hour Standing to cool Heat gently in an electric furnace 800 C 2 hours Standing to cool Desiccator Measure the mass to the order of 0 1 mg Scheme 1 Flow sheet for total sulfur content in fertilizers 31 5 10 12 2 3 1 m
315. nd labels JIS Q 0031 2002 E 8 FAMIC lt http www famic go jp ffis fert sub9 html gt 55 9 ISO 5725 6 1994 Accuracy trueness and precision of measurement methods and results Part 6 Use in practice of accuracy values JIS Z 8402 6 1999 6 10 Thomas Linsinger Comparison of a measurement result with the certified value European Reference Materials application note 1 European Commission Joint Research Centre Institute for Reference Materials and Measurements IRMM 2010 lt http www erm crm org ERM_products application_notes application_note_1 Documents erm_application_n ote 1 english rev3 pdf 122 Vol 7 2014 Long term Stability Evaluation of Fertilizer Certified Reference Materials fo
316. o hozen_type h_dozyo pdf chi4 pdf gt 12 Perkin Elmer 13 2001 14 46 6 24 47 24 8 6 22 2012 15 p 215 219 1997 16 Bland Altman pH 83 564 573 2012 17
317. onium sulfate 10 1 0 0343 0 0015 4 5 0 0040 11 6 1 74 1 Number of laboratories where p number of laboratories retained after outlier removed and 9 number of outliers 2 Grand mean value n The number of participating testing laboratoried p X The number of times of repetition 2 3 Mass fraction 4 Standard deviation of repeatability 5 Relative standard deviation of repeatability 6 Standard deviation of reproducibility 7 Relative standard deviation of reproducibility 8 Horwitz ratio of reproducibility 18 Vol 7 2014 Table 4 2 Statistical analysis of collaborative study results for ammeline No of labs Mean 6 2 sg Sample 1 3 3 RSD i 3 Rope HorRat p q 96 96 96 96 96 Calcium cyanamide 1 9 2 1 60 0 02 1 3 0 06 3 8 1 02 Calcium cyanamide 2 10 1 0 105 0 001 1 3 0 002 2 3 0 41 A qued 9 2 0 629 007 43 0 023 37 0 86 containing calcium cyanamide Compound fertilizer 11 0 0 195 0 004 2 1 0 009 4 5 0 87 Ammonium sulfate 10 1 0 0346 0 0013 3 7 0 0024 6 9 1 04 1 8 Refer to the footnote of Table 4 1 Table 4 3 Statistical analysis of collaborative study results for ammelide No of labs Mean s RSDD sre RSD 8 Sample D 3 3 3 HorRat p q Calcium cyanamide 1 9 2 1 10 0 02 2 1 0 08 7 6 1 92 Calcium cyanamide 2 11 0 0 361 0 008 2 2 0 023 6 5 1 39 d ded Ed 9 2 0188 0004 22 0014 75 1 46 containing Calcium cyanamide Compound fertilizer 11 0 0 7
318. ose of determination of cyanuric acid were reported 0 105 1 15 and 6 8 13 2 96 respectively These results indicated that this method has acceptable precision for determination of melamine ammeline ammelide and cyanuric acid in this density range The mean values and the RSDr of determination of ammelide in ammonium sulfate were reported 0 0345 and 16 1 96 respectively Those of determination or cyanuric acid in ammonium sulfate were reported 0 0365 and 18 3 96 respectively These results didn t indicate that this method has acceptable precision for determination of ammelide and cyanuric acid in this density range Key words melamine ammeline ammelide cyanuric acid calcium cyanamid fertilizer HPLC collaborative study Research Report of Fertilizer 7 Collaborative Study 10 21 2014 22 Vol 7 2014 3 ARRA FAMIC 2 JE
319. phosphoric acid T P2Os total potassium T K5O total calcium T CaO total copper T Cu total zinc T Zn organic carbon O C arsenic As cadmium Cd mercury Hg nickel Ni chromium Cr and lead Pb The monitoring long term stability was evaluated by a statistical analysis of the results of monitoring stability examination on the chemical analysis of the stock CRMs The data was performed a statistical analysis in reference to ISO Guide 35 2006 It show evidence that there were no need to update the certified value and its uncertainty From these results of the statistical analysis the all certified values of the CRMs of high analysis compound fertilizer FAMIC A 10 and ordinary compound fertilizer FAMIC B 10 were stable for three years and two months after preparation In addition composted sludge fertilizer FAMIC C 12 had little examination number of times but was the same It is compared the certification level with the measurements of CRMs by an introduced evaluation method in ERM Application Note 1 by reference The CRMs were expected to be useful for the quality assurance and the quality control in the analysis of major components and harmful elements in compound fertilizers Key words certified reference material CRM compound fertilizer composted sludge fertilizer major component harmful elements ISO Guide 31 ISO Guide 35 long term stability monitoring examination Research Report of Fertilizer 7 105 122 2
320. r Determination of Major Components and Harmful Elements High Analysis Compound Fertilizer FAMIC A 10 and Ordinary Compound Fertilizer FAMIC B 10 and Composted Sludge Fertilizer FAMIC C 12 Shigeyuki INABA Yasuharu KIMURA Taku FUJITA Keisuke AOYAMA Kouhei ITOU Masanori HASEGAWA and Yuji SHIRAI Food and Agricultural Materials Inspection Center Kobe Regional Center Food and Agricultural Materials Inspection Center Fertilizer and Feed Inspection Department Food and Agricultural Materials Inspection Center FAMIC has performed long term stability examinations to confirm shelf life of fertilizer certified reference materials CRMs high analysis compound fertilizer FAMIC A 10 ordinary compound fertilizer FAMIC B 10 and composted sludge fertilizer FAMIC C 12 for analysis of major components and harmful elements FAMIC A 10 is certified for the contents of total nitrogen T N ammonium nitrogen A N citric acid soluble phosphorus C P205 water soluble potassium W K2O citric acid soluble magnesium C MgO citric acid soluble manganese C MnO and citric acid soluble boron C B505 FAMIC B 10 is certified for the concentrations of ammonium nitrogen A N neutral citrate soluble phosphorus S P20s water soluble phosphorus W P2Os water soluble potassium W K2O arsenic As cadmium Cd lead Pb nickel Ni and mercury Hg FAMIC C 12 is certified for the concentrations of total nitrogen T N total
321. ration dry matter 3 It is no significantly different for standard plot t test 5 of both sides levels of significance the harvest is n 2 the cadmium quantity of cadmium uptake is n 4 2X2 repetition x number of samples 4 It is significantly different for Standard plot t test 5 of both sides levels of significance the cadmium concentration is n 4 2x2 repetition x number of samples H 51 2 0 1 mol L HCI Cd 1 mol L pH 7 0 Cd pH EC Table 8 0 1 mol L HCI Cd 0 21 mg kg 0 17mg kg THV 0 05 1 mol L HE pH 7 0 Cd 0 038 mg kg 0 032 mg kg CH 0 05 Table 8 Characteristics of soil used in this study Unit Test plot 1 Test plot 2 Average t test lt Sludge fertilizer application plot AP gt 0 1 mol L HCLCd mg kg 0 20 020 0 21 021
322. re 2 40 74 7 5 2 97 5 2 6 72 7 8 6 Composted sludge 1 000 823 15 8 6 87 900 24 fertilizer 400 91 4 4 5 95 1 2 0 105 0 3 6 containing pig manure 40 765 42 895 10 2 92 7 24 a Mean Value n 3 b Relative standard deviation Table 6 Calculated LOQ and LOD values ug kg Agricultural a b d Sample Reid Spiked level Mean s LOQ LOD Clopyralid 20 14 9 1 3 13 5 Cattle manure compost Aminopyralid 20 14 0 1 1 11 4 Picloram 20 16 5 0 8 8 3 Composted sludge Clopyralid 20 15 1 1 4 14 5 fertilizer Aminopyralid 20 14 8 1 1 11 4 containing cattle manure Picloram 20 18 9 1 4 14 6 a Mean Value n 7 b Standard deviation c sxl0 d sx2xt n 1 0 05 4 8 Vol 7 2014 1 0 ng mL 100 ng mL 0 0025 ng 0 5 ng 2 2 2 1
323. reproducibility TH A and trueness estimates in measurement uncertainty estimation JIS Z 8404 1 2006 1 14 ISO 31 0 1992 Quantities and units Part 0 General principles Annex B Informative Guide to the rounding of numbers JIS Z 8401 1999 15 BAEZ 2011 EE JE FAMIC A 10 FAMIC B 10 FAMIC C 09 5 90 100 2012 EY 104 Vol 7 2014 Preparation of Certified Reference Material CRM for Determination of Major Components High anlysis Compound Fertilizer FAMIC A 13 Shinichi KASHIMA Toshiharu YAGI Hisanori ARAYA Satono AKIMOTO Aiko YANO Mariko FUJITA Yoshimi HASHIMOTO Toshiaki HIROI Yuji SHIRAI and Akira KUBO Food and Agricultural Materials Inspection Center Fer
324. rmined on 1 5 soil water suspensions with a glass electrode n 1 4 Soil electrical conductivity determined on 1 5 soil water suspensions with an electricalconductivity meter n 1 5 Content in the dry matter average n 2 6 Mass fraction 7 The year when the study was designed to evaluate the effects of sluge fertilizer aplications on soil intended for long term use 8 The year when this study was conducted 2 2 1 2 ao 3 2 1 3 500 kg 10 a 30 Table 6 pu
325. rochloric Acid Treated Combustion Method A Collaborative Study Aiko YANO and Yuji SHIRA Food and Agricultural Materials Inspection Center Fertilizer and Feed Inspection Department Now Fukuoka Regional Center Food and Agricultural Materials Inspection Center Fertilizer and Feed Inspection Department A Collaborative study was conducted to evaluate hydrochloric acid treated combustion method for determination of organic carbon in sludge fertilizer and compost Analytical sample was treated with dilute hydrochloric acid and dried up before measurement of organic carbon by total nitrogen and total carbon analyzer Five types of test materials Human waste sludge fertilizer Industrial sludge fertilizer Calcined sludge fertilizer Composted sludge fertilizer and Compost were sent to 9 laboratories in a blind duplicate design After removal of outlier caused by a failure to follow the method Cochran and Grubbs tests were conducted and a pair was indicated to be Cochran outlier in Human waste sludge fertilizer Statistical analysis was conducted for data retained after removal of the outliers Mean values were in the range of 9 45 to 38 20 mass fraction and the repeatability relative standard deviation RSD and the reproducibility relative standard deviation RSDs ranged from 0 2 to 3 7 1 8 to 4 6 respectively These results indicated that this method was validated for determination of organic carbon in sludge fertilizer
326. s NIQR and relative standard deviations RSDs for reproducibility of S SiO obtained by proficiency testings were 28 25 36 15 96 0 48 96 0 87 96 and 1 3 96 3 1 96 respectively These results indicated that this method performance characteristic was available in establishing criteria for a determination method of S SiO Key words criteria approach silicic acid potassium fluoride method Testing Methods for Fertilizers Research Report of Fertilizer 7 123 130 2014 Hd FU 131 HT anb on Zul R 11 7 lt 1 ISO IEC 17025 2005 JIS Q 17025 2005 ISO IEC 17025 ZS
327. s HLB 6cc 200 mg 6 AS ONE MCD 2000 7 Waters 4 1 5 00 g 200 mL 4 w v96 1 mL 99 mL 30 50 mL 3 000 rpm 1 300xg 2 Si 5 mL 5 mL 50 mL mL 0 04 w v 1 1 5 mL 2 3 fe 52 5 mL 1 120 5 mL 40 C 5 mL 1 11 3
328. sium W MgO citric acid soluble manganese C MnO citric acid soluble boron C B203 total arsenic T As and total cadmium T Cd were analyzed using a compound fertilizer sample Acid soluble silicon S S1O alkalinity AL and citric acid soluble magnesium C MgO were analyzed using a silicate slag fertilizer sample Two homogenized samples were sent to the participants From the 143 participants which received a compound fertilizer sample 52 136 results were returned for each element From the 82 participants which received a silicate slag fertilizer sample 60 79 results were returned for each element Data analysis was conducted according to the harmonized protocol for proficiency testing revised cooperatively by the international standardizing organizations IUPAC ISO and AOAC International 2006 The ratios of the number of z scores between 2 and 2 to that of all scores were 77 96 100 and the results from the satisfactory participants were almost normally distributed The mean and the median of all elements slightly differed from each other The median NIQR plots were distributed near Horwitz curve for each element and the HorRat values were less than 2 0 for all elements except for 3 elements Where more than 7 results were returned no significant distribution difference was observed between the different methods used except for 3 elements W K 0 T Cd and AL Vol 7 2014 94 Key words
329. sphate Compound Compound Compound ID fertilizer mixture 1 fertilizer mixture 2 fertilizer 1 fertilizer 2 fertilizer 3 A 25 18 24 93 33 60 33 66 29 80 29 42 32 660 32 42 15 66 15 46 B 25 25 25 14 34 57 34 53 30 08 30 14 33 55 33 72 15 83 15 73 C 25 08 24 99 34 32 34 26 29 98 30 04 33 19 33 36 15 63 15 69 D 25 03 24 72 34 86 34 79 30 99 30 89 33 78 33 92 15 80 15 93 E 24 58 24 95 34 27 34 28 29 98 29 85 32 85 32 74 15 74 15 39 F 24 36 24 49 34 49 3422 30 08 29 89 33 31 33 41 15 92 16 01 G 25 12 25 09 34 49 35 39 30 47 30 46 33 78 33 50 15 59 15 61 H 25 37 25 60 34 86 35 26 31 51 31 24 33 55 33 76 16 11 16 03 1 Laboratory identification 2 Outlier of Cochran 40 Vol 7 2014 3 s RSD ss m RSDr HorRat Table 3 15 76 34 50 96 5 BOO sp 0 11 0 26 0 21 0 60 RSD RSD 0 4 0 7 PRU 1 3 96 2 0 HorRat 0 53 1 09 2
330. t C2014 3 ze PA v FAMIC B 10 gt 7 9 1x UE D aoe cma kd f PM J 4M FAMIC i Ct et GERE OAK 2 FAMIC A B 2010 7 H 9 A 2011 7 9 A 2012 4 A 2012 7 9 A 2012 12 H 2013 1 H 2013 4 H 5 2013 10 11 Host 7 C 2012 8 10 H 2013 4 H 5 2013 10 11 3 A B C 1 2 A B As Cd Hg Ni Pb C MnO C B O 3 2 C T Cu TZn 3
331. t exchanging aim yield kg 10 a to 4 m 4 Fresh weight index of sludge fertilizer application plot when standard plot assume 100 5 Standard deviation n 2 2 repetition 2 pH EIE pH OF E Fig 2 pH 6 0 6 7 BKE pH pH 6 0 pH pH pH 29 pH b
332. tandard deviation of reproducibility 7 Relative standard deviation of reproducibility 8 Horwitz ratio of reproducibility 3 RSD se BHP iP EL J ake E 0 07 0 76 HU E 9 45 Jp HorRat HL F RSD HorRat Table 4 38 20 96 THN 0 2 3 7 4 d 26 Vol 7 2014 0 38 0 94 1 8 4 6 4 9 3 10
333. tilizer and Feed Inspection Department Food and Agricultural Materials Inspection Center Fertilizer and Feed Inspection Department Now Ministry of Agriculture Forestry and Fisheries Food Safety and Consumer Affairs Bureau Food and Agricultural Materials Inspection Center Fertilizer and Feed Inspection Department Now Fukuoka Regional Center Food and Agricultural Materials Inspection Center FAMIC has developed a certified reference material CRM high analysis compound fertilizer FAMIC A 13 for analysis of major components FAMIC A 13 was certified for the contents of total nitrogen T N ammonium nitrogen A N citric acid soluble phosphoric acid C P2O3 water soluble potassium W K5O citric acid soluble magnesium C MgO citric acid soluble manganese C MnO and citric acid soluble boron C B2O3 The certified values were obtained from a statistical analysis of the results of a collaborative study on the chemical analysis of the candidate for CRM Ten laboratories participated in this study In a statistical analysis of data which were reported from participants outliers were removed by Cochran test and Grubbs test followed by the usual statistical procedure The CRMs were expected to be useful for the quality assurance and the quality control in the analysis of major components in high analysis compound fertilizer Key words certified reference material CRM high analysis compound fertilizer major component ISO Guide
334. tivated soil The error bar indicating the standard deviation 56 Vol 7 2014 Table 12 Change of the 0 1 mol L HCLCd density of ruins soil Ap SP 3 t test PRE of singt 5 Year Season Test crops ee TRETEN DAS between the mg kg mg kg occ AP sp 2009 Start 0 19 0 01 0 20 0 02 ns E 2009 Summer Carrot 0 21 0 01 0 21 0 02 n s aa 2009 Winter Spinach 0 20 0 003 0 18 0 01 n s 2010 Summer Spmach 0 19 0 01 0 17 0 02 n s 2010 Winter Qing gengcai 0 18 0 02 0 18 0 01 n s 0 55 0 20 2011 Summer Turnip 0 19 0 004 0 18 0 01 n s 0 41 0 11 2011 Winter Spinach 0 20 0 01 0 17 0 01 significance 0 63 0 03 2012 Summer Carrot 0 19 0 005 0 15 0 01 significance 0 41 0 01 2012 Winter Spinach 0 21 0 01 0 17 0 01 significance 0 98 0 01 9 2013 Summer Carrot 0 20 0 004 0 16 0 01 significance 0 89 0 002 8 1 Content in the drying soil 2 Sludge fertilizer application plot 3 Standard plot 4 The p value which calculated from dispersion analysis for linear regression by examination start of each examination plot 5 Standard deviation n 4 2X2 repetition X number of samples 6 It is no significantly different for Processing examination section t test 5 of both sides levels of significance n 4 2x2 repetition x number of samples 7 It js significantly different for Processing examination section t test 5 of both sides lev
335. to sample including repeatability 9 F value calculated based on analysis of variance ANOVA 10 F critical value F 9 10 0 05 3 02 F 8 9 0 05 3 23 2 Table 3 IUPAC AOAC 1 1 Cochran Grubbs Cochran 1 MIELE AC J P E MEUELR UHER ORR RORE HRR 25 Table 3 Individual result of organic carbon in sludge fetilizer and compost mass 96 ES Calc ined sludge Industrial sludge Compost Human waste Composted sludge ID fertilizer fertilizer sludge fertilizer fertilizer A
336. ure amp Appl Chem 67 2 331 343 1995 10 AOAC OFFICIAL METHODS OF ANALYSIS Appendix D Guideline for Collaborative Study Procedures To Validate Characteristics of a Method of Analysis AOAC INTERNATIONAL Gaithersburg 2005 H 11 Thompson M Recent trends in inter laboratory precision at ppb and sub ppb concentrations in relation to fitness for purpose criteria in proficiency testing Analyst 125 385 386 2000 12 Codex Alimentarius CODEX ALIMENTARIUS COMMISSION PROCEDURAL MANUAL Twentieth edition p66 2011 EE Te BER BIE 35 L Testing Method of the Total Amount of Sulfur Content as Sulfur Trioxide A Collaborative Study Shin ABE Chika SUZUKT and Yuji SHIRAT Food and Agricultural Materials Inspection Center Sendai Regional Center Now Fertilizer and Feed Inspection Department Food and Agricultural Materials Inspection Center Sendai Regional Center Food and Agricultural Materials Inspection Center Fertilizer and Feed Inspection Department A collaborative study was conducted to evaluate the applicability of the method validation of gravimetric analysis for determination of sulfur content in sulfur and its compounds as fertilizer Sulfur in fertilizer was dissolved in potassium hydroxide ethanol solution and oxidized to sulfate ion by adding hydrogen peroxide The precipitation of barium sulfate was generated by adding barium chloride solution to the

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