Achieving ISO17025 Accreditation

For Au Assay by ICPICP-OES

Using AuAu-Reference Materials
Hiroshi Sawai
TKG Laboratory Center
International
Standardisation Office
TANAKA KIKINZOKU KOGYO K.K.

Copyright TANAKA KIKINZOKU KOGYO K.K. All Rights Reserved.

The LBMA Assaying & Refining Seminar

7-8 March 2011

Overview
1 Tanakas Role in LBMA RM Project
2 Assay Procedure
3. Points for the Procedure
4. What is ISO/IEC 17025 ?
5 Benefits of Achieving ISO17025 Accreditation
6 Role of LBMA RMs in TKKs Achievement of
Obtaining ISO17025 Accreditation
7. Evaluation for Assay
8Uncertainty
9. Conclusion
TANAKA KIKINZOKU KOGYO K.K.

Tanakas

Tanakas Role in LBMA RM Project

1. Member of the Steering Committee
(with RCM, Metalor SA, Great Wall
WallRand Refinery and Umicore)

2. Au
Au--RM Project
*Manufacturer
*Assayer for derivation
of certificated value
3.

Ag
Ag--RM Project
*Assayer for derivation
of certificated value

Copyright TANAKA KIKINZOKU KOGYO K.K. All Rights Reserved.

The LBMA Assaying & Refining Seminar

7-8 March 2011

2. Assay Procedure for Gold Sample

Adding Acid

Liquefaction

(HCl & HNO3)

By

Weighing

Heat Block

Make up
Volume to
Level
Required

Measurements

By
ICP-OES

Copyright TANAKA KIKINZOKU KOGYO K.K. All Rights Reserved.

Make up Standard Solution

+
Preparation

Preparation

of

of

the Au

mixed metal

mother
solution

standard
solution

Make up standard
solution
for ICP
measurement

Copyright TANAKA KIKINZOKU KOGYO K.K. All Rights Reserved.

The LBMA Assaying & Refining Seminar

7-8 March 2011

3. Points for the Procedure

Concerning the procedure, the main points are as
follows:
1 The concentration of gold and acid in the sample
1.
solution must be the same as in the standard solution.
2. In order to avoid evaporation of acid during
dissolution, samples are heated in sealed vessels.
3. To pprevent errors due to the contamination of the
standard solution with other metals, the impurities in
the commercial standard solutions should be
carefully analysed.
Copyright TANAKA KIKINZOKU KOGYO K.K. All Rights Reserved.

4.What is ISO/IEC 17025 ?

ISO/IEC 17025 is the main standard used by testing and
calibration laboratories.
O i i ll it was started
Originally
t t d in
i order
d to
t provide
id assurance
about the accuracy of assaying or analysis carried out by
accredited laboratories, and thus avoiding the need for
additional assays.
The two main sections in ISO/IEC 17025 are
Management Requirements and Technical Requirements.
Requirements
Technical requirements include factors which determine
the correctness and reliability of the tests and calibrations
performed in the laboratory.
laboratory.
Copyright TANAKA KIKINZOKU KOGYO K.K. All Rights Reserved.

The LBMA Assaying & Refining Seminar

7-8 March 2011

5. Benefits of Achieving ISO17025

Accreditation
In the accredited Assay range
1.
2.
3.

The reliability of your assaying will

be recognised internationally.
Applying for ISO17025 accreditation will
i
improve
your assaying
i ability.
bili
Your customer will have increased
confidence in your assaying results.

Copyright TANAKA KIKINZOKU KOGYO K.K. All Rights Reserved.

6. Role of LBMA RMs in TKKs Achievement of

Obtaining ISO17025 Accreditation ?
1. To achieve ISO17025, you must prove that your
assay results match the international standards.
2. However, before the LBMALBMA-RM, there were no reliable
international standards for gold and silver.
3. LBMA
LBMA--RMs are the first standards to have been
produced by means of a collaborative international effort.
4. Comparing with LBMA RM, your assay ability can be
judged using appropriate statistical methods.
5. For achieving ISO17025 Accreditation, use of the LBMA
RMs is the most effective means of producing a
trustworthy assay.
Copyright TANAKA KIKINZOKU KOGYO K.K. All Rights Reserved.

The LBMA Assaying & Refining Seminar

7-8 March 2011

7.

Evaluation for Assay Ability

En LABREF/ULAB2UREF20.5
LABAssay by LaboratoryTKK Assay result
REFBasis by Reference LBMA Certified
ULABUncertainty at LaboratoryTKKs value
UREF Uncertainty at Reference LBMA s value

-1 < En < 1

Good assay ability

En < -1, En >1

Bad assay ability

Copyright TANAKA KIKINZOKU KOGYO K.K. All Rights Reserved.

8. Uncertainty
Calculation of the uncertainty is most
important item to get the accreditation of
ISO17025.
ISO17025
Assay results are given from many process.
So at first, we must calculate uncertainty at
each process.
Then final uncertainty is calculate by of each
uncertainty
Copyright TANAKA KIKINZOKU KOGYO K.K. All Rights Reserved.

The LBMA Assaying & Refining Seminar

7-8 March 2011

Certificate of LBMA AuAu-RMs

Element Concentrations, mg/kg
AuRM1
Ag
Al
As
Bi
Ca
Cr
Cu
Fe
Mg
Mn
Ni
Pb
Pd
Pt
Rh
Sb
Se
Si
Sn
Te
Ti
Zn

20.0
9.6
14.5
30.4
9.6
9.4
13.5
10.6
30.1
9.7
9.8
9.8
9.7
10.3
73
7.3
35.7
11.8
9.4
9.7
40.7
10.5
10.3

0.8
0.8
1.0
1.5
1.1
0.6
2.7
1.1
1.9
0.4
1.0
1.8
0.6
1.1
06
0.6
1.6
2.9
1.6
1.1
2.6
0.9
1.2

AuRM2
99.6
28.3
47.1
9.7
28.0
27.7
31.6
30.1
9.9
28.2
29.2
28.9
29.2
30.2
39 6
39.6
11.3
37.4
28.0
29.4
12.0
31.6
31.4

AgRM1
Al
As
Au
Bi
Cd
Cr
Cu
Fe
Mg
Mn
Ni
Pb
Pd
Pt
Rh
Sb
Se
Si
Sn
Te
Zn

5.6
1.8
2.8
0.8
2.6
2.2
2.4
2.2
0.9
1.5
2.6
2.4
1.3
2.1
24
2.4
1.6
2.8
3.8
1.8
3.2
1.3
2.3

7.9
19.0
6.1
7.3
8.0
62.9
30.2
22.4
13.9
8.9
66.1
37.5
5.2
5.5
13.4
4.5
23.0
10.0
49.2
4.7
26.9

1.2
2.4
0.8
1.1
0.9
6.0
2.3
1.9
1.3
0.6
4.2
1.1
0.4
0.7
5.2
0.4
1.6
2.6
6.3
0.5
1.5

AgRM2
61.8
5.5
26.2
40.8
23.5
8.8
110.5
15.7
49.3
16.1
10.6
5.6
23.1
20.9
4.6
23.6
8.6
54.6
4.5
38.1
5.2

8.1
1.0
1.5
3.0
1.2
1.2
2.6
2.2
4.6
0.9
2.5
1.0
1.7
4.2
1.3
2.4
0.6
8.2
0.6
3.5
0.5

Copyright TANAKA KIKINZOKU KOGYO K.K. All Rights Reserved.

LB M A R M -1
Elem ents
Ag
Al
As
Bi
Ca
Cr
Cu
Fe
Mg
Mn
Ni
Pb
Pd
Pt
Rh
Sb
Se
Si
Sn
Te
Ti
Zn

C oncentration
m g/kg
LB M A B asis TK K A ssay
20.0
19.7
9.6
9.1
14.5
14.7
30.4
30.0
9.6
9.3
9.4
9.6
13.5
13.4
10.6
10.8
30.1
30.1
9.7
9.5
9.8
10.1
9.8
10.2
9.7
9.7
10.3
10.3
7.3
7.4
35.7
35.7
11.8
10.5
9.4
8.5
9.7
9.9
40.7
43.0
10.5
10.9
10.3
10.9

D if
0.3
0.5
0.2
0.4
0.3
0.2
0.1
0.2
0.0
0.2
0.3
0.4
0.0
0.0
0.1
0.0
1.3
0.9
0.2
2.3
0.4
0.6

U ncertainty(k=2)
m g/kg
LB M A
TKK
0.8
0.8
0.8
0.2
1.0
0.9
1.5
1.1
1.1
0.2
0.6
0.2
2.7
0.3
1.1
0.2
1.9
0.5
0.4
0.2
1.0
0.2
1.8
0.5
0.6
0.2
1.1
0.3
0.6
0.1
1.6
0.9
2.9
0.8
1.6
0.4
1.1
0.5
2.6
1.5
0.9
0.1
1.2
0.4

En
-0.3
-0.6
0.1
-0.2
-0.3
0.3
0.0
0.2
0.0
-0.4
0.3
0.2
0.0
0.0
0.2
0.0
-0.4
-0.5
0.2
0.8
0.4
0.5

Copyright TANAKA KIKINZOKU KOGYO K.K. All Rights Reserved.

The LBMA Assaying & Refining Seminar

7-8 March 2011

Conclusion
1. TKK achieved ISO17025
Accreditation for Au Assay by ICP
OES.
OES
2. To obtain this accreditation, the
reliability of your assay will be
evaluated from an international
viewpoint.
3. Using of LBMA RM is the most
effective method of achieving accreditation.
Copyright TANAKA KIKINZOKU KOGYO K.K. All Rights Reserved.

Thank you for your

kind attention
L t join
Lets
j i
17025 world

The LBMA Assaying & Refining Seminar

7-8 March 2011