FAMIC-C-21 Certificate(Sample)

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Note:This is unofficial translation. Only the original Japanese texts have effectand the translation is to be used solely as reference material.
This center assumes no responsibility whatever for any direct, indirect, special,incidental, consequential damages and any other damages resulting from the useof this contents.

Certified Reference Material Fertilizer C
Composted Sludge Fertilizer

FAMIC-C-21No. +++Certificate (Sample)
This reference material is produced by grinding composted sludge fertilizer specified in the officialspecifications of ordinary fertilizers 1) to be homogenized. It can be used for quality control of theanalysis results and for the validation of the analysis method, etc., in the quantitation of the maincomponents, organic carbon, and harmful components of composted sludge fertilizer analyzed by theTesting Method for Fertilizers.
[Certified value]
The certified value (wet concentration) of the reference material and its uncertainty is as shown below.
The uncertainty of the certified value is expanded uncertainty multiplying the standard uncertainty,
which is obtained in a collaborative study to determine the certified value, by the coverage factor (k= 2). The number of digits to be expressed is up to the order of the minimum limit of quantificationin the Testing Methods for Fertilizers, etc.
Table 1 Certified Value
Content
Expanded Uncertainty
Component(µ)(U95% )
Mass Fraction (%)
Mass Fraction (%)
Total nitrogen (T-N) Combustion method

4.11

0.02

Total nitrogen (T-N) Kjeldahl method

3.8

0.1

Total phosphorus (T-P 2 O 5 )

5.29

0.04

Total potassium (T-K 2 O)

0.530.02

Total calcium (T-CaO)

4.16

0.08

Organic carbon (O-C)

27.0

0.20

Content(µ)(mg/kg)Expanded Uncertainty(U95% )
(mg/kg)Total copper (T-Cu)

447

8

Total zinc (T-Zn)

1340

14

Arsenic (As)

7.3

0.6

Cadmium (Cd)

2.0

0.1

Mercury (Hg)

0.61

0.02

Nickel (Ni)272

Chromium (Cr)

312

Lead (Pb)23

1Component

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FAMIC-C-21 Certificate(Sample)

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[Analytical methods]
Analysis is according to the Testing Methods for Fertilizers 2). Analytical methods for respective
components are shown below:
Table 2 Analytical Methods
Testing Methods for Fertilizers

Component

Total nitrogen(T-N)

4.1.1.b

Combustion method

4.1.1.a

Kjeldahl method

Minimum amountof Analytical
Sample for 1Analysis
0.05 g - 0.5 g
2.5 g

Total phosphorus(T-P 2 O 5 )4.2.1.a Ammonium vanadomolybdate absorptiometric analysis

Total potassium(T-K 2 O)

4.3.1.a Flame atomic absorption spectrometry or flame
photometry

5g

Total calcium(T-CaO)4.5.1.a

Flame atomic absorption spectrometry5g

4.11.1.aDichromate oxidation

0.05 g4.11.1.bCombustion method0.05 g4.10.1.aFlame atomic absorption spectrometry

5g

Organic carbon(O-C)
Total copper(T-Cu)

2.5 g - 5 g

4.10.1.b ICP Optical Emission Spectrometry

5g

4.9.1.a

Flame atomic absorption spectrometry

5g

4.9.1.b

ICP Optical Emission Spectrometry

5g

5.2.a

Hydride generation atomic absorption spectrometry

1g-2g

5.2.b

Silver diethyldithiocarbamate absorption spectrometry

1g–2g

5.3.a

Flame atomic absorption spectrometry

5g

5.3.bICP Optical Emission Spectrometry

5g

5.1.a

Cold vapor atomic absorption spectrometry

1g

5.4.a

Flame atomic absorption spectrometry

5g

5.4.b

ICP Optical Emission Spectrometry

5g

5.5.a

Flame atomic absorption spectrometry (fertilizers
containing organic matters)

5g

5.5.d

ICP Optical Emission Spectrometry

5g

Lead(Pb)

5.6.a

Flame atomic absorption spectrometry

5g

5.6.b

ICP Optical Emission Spectrometry

5g(Referenceinformation)
Moisture (H 2 O)

3.1.a

Loss on drying method with drying apparatus*

5g

3.1.b

Loss on drying method by moisture analyzers**

5g

Total zinc(T-Zn)
Arsenic(As)Cadmium(Cd)Mercury(Hg)
Nickel(Ni)Chromium(Cr)* ： 100 ℃ ± 2 ℃, 5hours** ： Dry at 100 ° C until constant weight (mass loss 1 mg / 90 seconds or 1 mg / 140 seconds or less)

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FAMIC-C-21 Certificate(Sample)

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For details of analytical methods for components shown above, see the “Testing Methods for
Fertilizers” disclosed in the website of the Food and Agricultural Materials Inspection Center.
URL for the above mentioned method: Testing Methods for Fertilizers
http://www.famic.go.jp/ffis/fert/obj/shikenho_2021.pdf[Method to determine the certified value]
A collaborative study by 14 laboratories was conducted to determine the certified value of thereference material in December, 2021. 3) 4)
The mean of the quantitation value in the collaborative study was determined as the certified value.
In the calculation of the mean, the Cochran test at the one-sided significance level of 1 % and theGrubbs test at the two-sided significance level of 1 % were conducted to exclude outliers.4)[Traceability]
The certified value of the reference material is the mean of the quantitation value in the collaborative
study conducted by the “Testing Methods for Fertilizers” , which was validated using a referencematerial and standard solution traceable to the specified reference material (national standard) basedon the Article 134 of the Measurement Law.
[Calculation of uncertainty]
The standard deviation of the total mean of the collaborative study is defined here as standard
uncertainty (u), which is calculated according to formula (a) using the repeatability standard deviation( ), reproducibility standard deviation ( R ), the number of laboratories (p) and the number ofrepetitions (n = 6) at each laboratory of the collaborative study. The uncertainty of certified value isexpanded uncertainty, which is obtained, after rounding the standard uncertainty (u) to one significant
digit, by multiplying the rounded standard uncertainty (u) by the coverage factor (k) (formula (b)),
and rounding the product off to the minimum limit of quantification of the “Testing Methods forFertilizers”. The coverage factor (k) is 2, which corresponds to a 95 % confidence interval for thenormal distribution. 5, 6)Standard[Attestation date]

uncertainty ( ) =2−2%) =×R

Expanded uncertainty (February 25, 2022

+2・・・（a）・・・（b）[Expiration date]
The expiration date of the reference material is the end of June 2026 under the storage conditions
shown below and unopened . Moreover, when change arises in the certified value by deterioration
unexpected in the term of validity etc., it will be published on the FAMIC website.
[Form]The reference material is powder that passed through a sieve of 500 μm aperture, and is sealed in anamber glass vial. The content is about 150 g.
[Homogeneity]
From 320 vials of a reference material candidate, 10 vials were sampled randomly to quantitate thecontent of the certified component in duplicate using one of the analytical methods listed in Table 2,3/7

FAMIC-C-21 Certificate(Sample)

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and one-way analysis of variance was duplicated × 10 samples. As a result, no significant
difference was observed between samples at the one-sided significance level of 5 %. The repeatability
relative standard deviation was 0.2 % to 5.9 %.
[Storage precautions]Store the reference materials at normal temperature (20 ℃±10 ℃) and protect them from direct
sunlight, high temperature and high humidity. After opening, make sure to close the inner lid, andstore sealed as much as possible.
[Usage precautions]
After using the reference material, do not leave the container open, and immediately close the innerlid.
The amount to be used in one analysis is shown in Table 2.
Moreover, the plants grown using this reference material are not to be served as food.
[Handling precautions]
Use the reference material for test only. Care should be taken to avoid injury when opening thecontainer.
After opening, if the reference material becomes contaminated or deteriorated, it cannot be used as acertified reference material.
[Manufacturing method]
This reference material was prepared in the following process using a commercial composted sludge
fertilizer produced by fermenting for 45 - 60 days after mixing human waste sludge, industrial sludge,
sewage sludge and food residue.
After drying about 100 kg of composted sludge fertilizer in a constant temperature dryer at 65 ℃ for
5 hours or more, pulverize it with an ultra centrifugal pulverizer until it passes through a sieve with
an aperture of 500 μm, homogenize, and then about 150 g brown Subdivided into glass bottles andsealed. Thereafter, sterilization by gamma irradiation was performed as a mold prevention measure.
[Reference information]
All of the certified value was for wet concentration. Moisture is tested by the loss on drying methodwith drying apparatus (Testing Methods for Fertilizers 3.1.a) and the loss on drying method bymoisture analyzer (Testing Method for Fertilizers 3.1.b) , and the moisture content by method isshown in Table 3.
The standard deviation of reproducibility, the standard deviation of repeatability, the drying matterconversion factor of a certified value and the number of effective data calculated from the results ofthe collaborative study to determine the certified value of the reference material are shown in Table
4 as reference.
In the joint test results, there was a difference in the average value between the Kjeldahl method andthe combustion method. Since this difference is that nitrate nitrogen contains a mass fraction of 0.36%(number of test rooms = 1, n = 3, phenolic sulfuric acid method (Testing Method for Fertilizers
4.1.3 .c) in the sample (Table 5), the certification value was set for each analysis method (Table 1) inthis certified standard material, so be careful when using this standard substance.

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FAMIC-C-21 Certificate(Sample)

Table 3

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Reproducibility Standard Deviation and Repeatability Standard Deviation
by method of Moisture (Reference Information)

ComponentMoisture(H 2 O) Loss on drying
method with drying apparatus
Moisture(H 2 O) Loss on drying
method by moisture analyzers

Numberoflaboratories(p (q))*

Reference Value(µ)
Mass Fraction(%)

Reproducibility
Standard Deviation( )Mass Fraction (%)

Repeatability
Standard Deviation( )Mass Fraction (%)

8 (1)

12.0

0.5

0.2

6 (0)

13.2

0.20.2* p=number of laboratories retained after outlier removed and (q)=number of outliers

Table 4 Reproducibility Standard Deviation, Repeatability Standard Deviation and Drying
Matter ( Loss on drying method with drying apparatus) Conversion Factor of Certified Value

MassFraction(%)

Reproducibility Standard
Deviation( )Mass Fraction(%)

Repeatability
Standard
Deviation( )Mass Fraction(%)

Certified
Value on a
Dry Moisture
Basis
MassFraction
(%)

9 (1)

4.11

0.02

0.02

4.67

9 (0)

3.8

0.17

0.09

4.32

Total phosphorus (T-P 2 O 5 )

12 (1)

5.29

0.07

0.04

6.01

Total potassium (T-K 2 O)

12 (0)

0.53

0.03

0.01

0.60

Total calcium (T-CaO)

9 (3)

4.16

0.120.07

4.7

Organic carbon (O-C)

10 (1)

27.0
CertifiedValue(µ)

0.2
Repeatability
Standard
Deviation( )(mg/kg)30.7

Component

Total nitrogen (T-N)
Combustion method
Total nitrogen (T-N)
Kjeldahl method

Number oflaboratories(p (q))*

Certified
Value(µ)(mg/kg)

0.4
Reproducibility Standard
Deviation( )(mg/kg)Total copper (T-Cu)

11 (2)

447

16

9515

Total zinc (T-Zn)

10 (3)

1340

35311543

Arsenic (As)

11 (0)

7.3

1.1

0.3

8.4

Cadmium (Cd)

11 (2)

2.0

0.06

0.04

2.3

Mercury (Hg)

12 (1)

0.61

0.05

0.03

0.71

Nickel (Ni)

13 (0)

273

132

Chromium (Cr)

13 (0)

313136

Lead (Pb)

11 (2)

2310.426Component

Number oflaboratories(p (q))** p=number of laboratories retained after outlier removed and (q)=number of outliers

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Certified
Value on a
Dry Moisture
Basis (mg/kg)

FAMIC-C-21 Certificate(Sample)

Table 5ship date：month, day, year

Nitrate nitrogen of this certified standard substanceComponent

Reference Value (µ) a)
Mass Fraction (%)

Standard Deviation (s)Mass Fraction (%)

0.360.002a) n=3b) Testing Method for Fertilizers 4.1.3.c Phenol sulfuric acid method

Nitrate nitrogen (N-N) b)[Laboratories in the collaborative study (in the Japanese syllabary order)]Japan Food Research Laboratories
Environment Research Center, Ltd.
Sumika Chemical Analysis Service, Ltd.
Nasu Kankyo Gijutsu Center Co., Ltd.
Hokuriku Environmental Science Institute Inc.
Kansai Branch, Japan Fertilizer and feed Inspection Association
Headquarters, Japan Fertilizer and feed Inspection Association
Kobe Regional Center, Food and Agricultural Materials Inspection Center
Sapporo Regional Center, Food and Agricultural Materials Inspection Center
Sendai Regional Center, Food and Agricultural Materials Inspection Center
Nagoya Regional Center, Food and Agricultural Materials Inspection Center
Fukuoka Regional Center, Food and Agricultural Materials Inspection Center
Headquarters, Food and Agricultural Materials Inspection Center
Nagasaki Agricultural and Forestry Technical Development Center[Acquisition of information]
Changing the certified value or the like, as well as notify the purchaser if there is significant revision,is posted on the website below.
It should be noted that, with respect to technical information on how such use of this standard is tobe referred to Annex "Using this certified reference substance".
URLs for the above website: http://www.famic.go.jp/ffis/fert/sub6.html[Reference specifications and literature]1) Public notice of the Ministry of Agriculture, Forestry and Fisheries: Subjects on theestablishment of official specifications for ordinary fertilizers based on the Fertilizer Control
Law, etc.: February 22, 1986, Notification No. 284 of the Ministry of Agriculture, Forestryand Fisheries, 1986. Final revision: June 14, 2021, Notification No. 1010, 2021.
2) Food and Agricultural Materials Inspection Center (FAMIC): Testing Methods for Fertilizers.
<http://www.famic.go.jp/ffis/fert/obj/shikenho_2018.pdf>

3)
4)
5)
6)

JIS Q 0035, Reference Materials – General and Statistical Principles for Certification, 2008.
JIS Z 8402-2, Accuracy (trueness and precision) of measured methods and values – Part II:
Basic methods to determine repeatability and reproducibility of standard measurement
methods, 1999.
Supervised by Kozo Iizuka: Guides for expression of accuracy in measurement, JapaneseStandards Association, 1996.
Japan Society for Analytical Chemistry, the supervisor of a translation: Quantifying
Uncertainty by Analytical Measurement, Japan Society for Analytical Chemistry (2013)

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FAMIC-C-21 Certificate(Sample)

7)

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Thompson, M., Ellison, S.L.R., Wood, R.: The International Harmonized Protocol for theProficiency Testing of Analytical Chemical Laboratories, Pure & Appl. Chem., 78 (1), 145~196(2006)[Contact center for the certified reference material]
Analysis Fertilizer and Soil Amendments Division, Fertilizer and Feed Inspection Department,Headquarters, Food and Agricultural Materials Inspection Center
Saitama New Urban Center, 2-1 Shin-toshin, Chuo-ku, Saitama-shi, Saitama (330-9731) Japan
TEL: (81) 50-3797-1856, FAX: (81) 48-601-1179
Website: http://www.famic.go.jp[Full name of certification director]
Food and Agricultural Materials Inspection Center
Administrative director Kiuchi Takeshi

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