80 KHoA HOC VA C ~ N G NGHE CONG HOA fi HOI CHU N G H ~ A VIET NAM TONG cvc TIEU CHUAN Dijc l@p - T ~ d o - H ~ n h phuc

oo LU'ONG CHAT L U ~ G

~ 6 : A ~ ~ , ~ / Q D - T D c Hh NGi, nghy 29 thring 8 nGm 201 4

q QUYET DJNH V$ vigc ban hanh V6n ban Kf thu$t Do l v h g Vigt Nam

TONG CUC TRU~NG TONG cuc T I ~ U CHURN DO L U N G CHAT LUWG

C5n clIr Lu$t Do lubng ngay 1 1 thing 1 1 n5m 20 1 1 ; .

C5n inu duy6t djnh s6 27120141QD-TTg ngay 04/4/20 14 cua Thu t u h g Chinh phu quy djnh chirc niing, nhiem vu, quy&n han va ccr ciu t6 chuc cua ,

~ 6 n ~ cpc Tiiu chuHn Do lubng c h i t luqng; Ciin ccir Th6ng tu s6 22/20 13/TT-BKHCN ngay 26 thang 9 nZim 20 13 cua

BG t r u h g B$ Khoa hoc va C6ng nghe quy djnh v& do lubng trong kinh doanh v h g va quan 19 chit lugng ving trang sirc, my nghe luu th6ng trin thj trubng;

C5n cu Q U ~ B ~ djnh 836lQD-TDC ngay 23/05/2011 cua ~ 6 n ~ cuc Tiiu chub Do l u h g c h i t luqng h u h g d8n trinh tu thu tuc x&y d m g ban hanh viin bA.n thuat do lubng Viet Narn;

Xit d& nghj cua Vu t n r h g Vu Do lubng,

DiBu 1. Ban hanh kim the0 quy6t djnh nay quy trinh hieu chuhn tam thbi thi6t bj huynh quang tia X (m) x L djnh ham luqng vang va quy trinh thir nghiem tam thbi chit chuhn hAm luqng vang.

Dieu 2. Giao Vien Do lubng Viet Nam thuc hien hi& c h u h thikt bi hujmh quang tia X (XRF) xac djnh ham luqng vang va thir nghiem chit chuhn ham luqng vang the0 quy djnh tai cic quy trinh nay d& chi djnh t6 chuc thir nghiem xac djnh ham luqng vang.

~ i 8 u 3. Q U ~ B ~ djnh nay co hieu luc k& tu ngay k9.

DiBu 4. Vu t n r h g Vu Do lubng, Vien tnrimg Vien Do lubng Viet Nam, Thu t r u h g cic t6 chuc, c6 nh&n co liin quan chiu trach nhiem t6 chlic, thqc hien Q U ~ B ~ dinh nay./.

Noi nhan: - Vi$n DLVN; TTKT 1,2,3; - TTDT; TT ThBng tin; - Luu: VT; DL.

9/

CHAT CHUAN HAM LUQNG VANG

- QUY TR~NH THO NGHIEM TAM THWI

Reference materials of gold - Temporary testing procedure

(Ban hdnh k h theo @ n h . / b $ k / ~ ~ - T ~ ~ n ~ d ~ .. d:-?I.tlirin g. .B. . .dm 2014

cua T6ng cgc f r u h g ~ 6 n g cgc TiLu chub Do l u h g ch& lupng)

chat chuan ham lwqng vang - Quy trinh thiv nghiem tam thbi ,

Reference materials of gold - Temporary testing procedure

1. Ph+m vi 5p dyng

Van ban @ thuijt nay quy djnh quy trinh do th13 nghiem phuc vu viec c h h g nhan ba chh chukn h8m luqng hpp kim vang (Au) vdi cac thdng s6 i j thugt va y2u ciu cu thk nhu sau:

#

- Gia tri nbng d$ kh5i luqng Au danh djnh: (30 + 99,99) %..

- VGt lieu'nin (matrix): Bac (Ag) vidhoac d6ng (Cu).

- Dugc su dung cung thikt bi hujlnh quang tia X (XRF) xac dinh h h luqng vang ,

d6 djdi @ ki6m tra d$ chinh x k cua thib b/ trong qua trinh hoat dong su dung h h g ngay.

2. Cac phCp thii nghiem

Phai ldn lugt tikn hanh cac phh$ thu nghiem ghi trong bing 1.

Bdng 1 I I

1 I Ki6m tra b2n ngoai 1 - 6.1

TT

3. Phwcmg tien thii nghiem

TCn phCp thii nghiem

2

3

Phumg tien thu nghiem phuc vy viec do thu nghiem co d$c tnmg @ thuat do l u h g ca b h dugc quy dinh trong bang 2 dudi diiy:

Theo di&u, mgcl cua quy trinh

Bdng 2 ,d

~ i & m tra @ thuat

Ki&m tra do l u h g

6.2

6.3

trinh

TT.1 Ten phlrmg ti@ thii. nghiem Dgc trlrng ky thu$t

do Ilrhg ccr b5n

1 .1

I

cac phCp the cua quy

chat chuin ham lugng .. vang (Au) tinh khikt dugc

chung nhan.

B$ chit c h u b ham lu(mg vang (Au) dupe c h ~ n g nhan tren nin bqc (Ag) va lho~c d h g (CU).

Gia tri ham lugng vang (Au) danh djnh: - 99,99 %.

Do khdng dam bao do: u 5 0,005 %

Gig tr/ ham lugng vang (Au) danh 1

6

djnh: (30 .+ 99) %.

Do khdng dam bao do: u 5 0,04 % 1 6

2 Phvang tien sir dyng cung vM chuhn

2.1

3

3.1

3.2

4. £lieu ki@n chung thb nghi@m

~ h i & t bi huynh quang tia X tan xa nang luqng micro (u-EDXRF)

3.3

Khi ti&n hlnh thir nghiem phhi dam bao clc dieu kien sau dPy:

Phqm vi do ham luqng A ~ :

(0 -+ 99,99) %

Phumg tien khac

- Nhi$t do: (1 0 +- 30) "C;

Phumg tien do nhiet do va 66 Bm m8i t k h g

Dung dich &a, lam sqch b&

Gang tay, panh gi!ip ch&t chuin hiun l u w g v h g , ao blouse,. . .

- Do dm khkhg khi: (30 t 80) %RH;

- Nhiet do: (0 +- 50) "C; Gia tr/ do chia: 1 "C. 4

- Do h kh6ng khi: (25 + 95) %RH; Gia trj do chia: 1 %RH.

I

5

- Khu vuc b6 tri thi&t bj c in trtinh tac dong b&n ngoai nhu: may phat dien, may han, song di$n tu, dien cao ap, . . .

Trubc khi tien hanh thu nghiem phai thuc hi&n cac c8ng viec chuin bj sau d6y :

mat chit k h u h ham luqng Dung m6i 1Bm sqch 16 can tuy$t d6i

C - Chon chuhn do l u h g vB phucmg tien thu nghiem the0 bang 2.

5

- BGt nguBn vh ven hlnh thikt bj the0 huhng d in cua n h i san xu& dk thi&t bi huynh quang tia X tan xq nang luqng micro (sau dPy ggi la thikt bj p-EDXRF) an djnh.

- Lam sach b& mat chht chuin ( d l chon the0 bang 2) vB cbc chht chuan cin thu nghiem: Trubc khi ti&n hinh thu nghiem, loqi b6 nhi&m ban tr@n bk mat chht chuin 4

Au bing can tuyet d6i, sau do rua lgi vbi nuirc tinh khikt (nubc cht 1 lin) va lam kh8 b& mat mau.

- Chon c lc dii do (n6u c6) quy djnh tren thiet b/ p-EDXRF.

- ~ h i & t lap dubng cong hieu chuan (calibration curve) tr&n thiet bi p-EDXRF vbi t6i thiku 05 chit chudn c6 ham luqng Au danh djnh phPn b6 dku trong khoing: (30 +- 99) % l i n luqt tu thhp d&n cao va 01 chht chuin co ham luqng Au danh djnh 99,99%.

6. ~ i 6 n hhnh thb nghi@m 6.1 ~ i i m tra b&n ngoai

Phai ki&m tra bEn ngoai the0 c k yeu cdu sau dPy:

- ~ i & m tra bing mit d&, xhc djnh su phu hcsp cba chit chuhn vang (Au) viri c L yEu cdu nhu: kich thuirc c h k chuhn, b& m$t chit chuhn phai phdng va n h h , ....

6.2 ~ i & m tra ky thugt

~ i k n hanh k i&d tra do chinh x ic cda thikt bi p-EDXRF:

+ Thuc hien ttbi thi&u 3 phCp do lien tikp vbi mdi c h k chuhn dii chon. Ghi kit

qua do dugc vao bien ban 6 phu luc 1.

+ Sai s6 gii , trung binh kkt qua do dugc viri gia trj chung hhgn cua chit chudn kh$ng duqc lirn han:

0,05 % d6i viri mgu c h u b Au co ham lugng tu 99 % tr6 lEn;

0,l % d6i viri mgu chuhn Au c6 ham lugng tu 80 % dkn 99 %;

0,i 5 % d6i viri mgu chuhn Au c6 ham lugng duiri 80 %.

6.3 ~ i 6 m tra do lvivng (Xdc e n h gia trj hhm l u p g vhng (Au)):

6.3.1 Thu nghiem xac djnh gia trj ham lugng vang (Au)

- Gia trj ham lupng vang c6a chit chuhn Au c h do thir nghiem dugc so sanh m c tikp

viri gia trj h h lupng ving ( tumg img) cua cac chit c h u b AU dugc chimg nh& (quy djnh trong bang 2) thbng qua thikt bj p-EDXRF c6 thbng s6 ky thugt phh hhgp viri yEu chu @ thuat quy djnh trong mpc 3.

- ~ i k n hanh do chit chudn AU dugc chimg nhgn t ~ i t6i thiku 5 vj tri khic nhau (mdi vi

tri do t6i thiku 1 l h ) phPn b6 d&u tren b& mat cda chit chuhn. Ghi kkt qua do dugc vao bien ban 3 phu luc- 1.

- ~ i k n h h h do chit chudn cdn thir nghiem tai t8i thiku 10 vj tri khac nhau (m8i vj tri

do t6i thiku 1 lib) phPn b6 d&u tren b& mat cua mgu thu nghiem (bao gbm c i dikm 6 trung t h ) . Ghi k h qua do duqc vao bien bin 6 phu luc 1.

6.3.2 Tinh toan gia trj ham lugng vang (Au)

- Gia trj ham lupng cua chht c h u b AU cPn thir nghiem dugc xac djnh nhu sau:

Trong 86:

.. [Au] : gia trj ham lupng Au cua chht c h u b ccn do thu nghiem, %; [AuIcrtM : gia trj ham lupng Au cua chht c h u b duqc chimg nhgn (theo GCN), %;

I;mul : gia trj do dugc tren chat c h u b cin chimg nhfin, %;

6.4.4 U'bc Ilrqng do khBng dam bao chudn mmir rong: ,

U = k.uc

k 18 he sb ph6 (k = 2 tlrong duong vbi xac suit tin cay P = 0,95).

7. XiY 19 chung

~ h h chuin vang (Au) sau khi thir nghiem n6u dat yyEu c iu quy d/nh the0 quy trinh

thu nghiem n8y duqc tip gihy chimg nhan k6t qua do thu nghiem kem the0 do

khang dam bao C6a phkp do. 1

Phu luc 1 ,

T6n cu quan thiY nghiem

Ten mau thu nghiem: .....................................................................................................

Ca sb sin xuiit: ....................................................... N5m sin xuiit: ..... I.. ..................... , I

Nuhc sin xuiit, : ............................................................................ : ................................ Dijc t- @ thuet: .......................................................................................................

Ca quan d i nghh/ thu nghiem: ........................................................................................ Phucmg phap thuc hien: ........................................................................ ~ i k u kien chung thu nghiem: .................................................................. Ngubi thuc hien: ................................................................................. Ten d m vi tqrc tiep thu nghiem:. .............................................................. Thbi gian thu nghiem tu .............................. d6n ....................................

1. ~ i e m tra b$n ngoiii:

2. Kern tra Q thuijt ( ~ i i m tra dij chinh XL cua thikt bj p-EDXRF):

Ham l u p g (%) :

Phtp do

I

Trung binh:

1 Sai sb cho phtp :

3. ~ i $ m tra do luimg (XPc djnh gia trj h im lupng vang):

- K B ~ qu8 do tren chit chuin Au qu6c gia:

- K B ~ qua do tr2n chht chudn Au c h thu nghiem:

Nguiri soat lgi Nguiri thvc hien .. '$4

. !$J :/-

..,.......

8

~ h h t chuin Au s6 :

Ham lugng (%) : .,

Phep do

1

2

3

4 ,

5

..... . Trung binh:

d

2. 1. 3.

2. 3. M ~ U SA:

Ham lugng (%) :

Phep do

1

2

3

4

5

6

7

8

9

10

..... Trung binh:

1. .......... n.

1

M ~ U chuhn vang (Au) - Quy trinh thu nghiem (Chirng nhgn) <

DLVN 113 : 20~03

Yeu cdu vk n$i dung va c k h trinh bay vv8 bAn ky thugt Do l u h g Vi&t Nam.

T H l h B! HUYNH QUANG TIA X (XRF) UC D!NH HAM LU'Q'NG VANG - QUY TR~NH HIEU CHUAN TAM THO1

X-ray fluorescence spectrometers - Temporary Calibration procedure

(Ban hhcinh k2m theo p y i t djnh . d ~ ~ ~ ~ D - ~ D ~ n g i y .. &$.thdn g..g...nrim 2014 cua T6ng cuc tru&ng T6ng cgc TGu chukn Do l u h g chkt lupng).

~ h i e t bj hupnh &ang tia X (XRF) x5c djnh h8m lulqng vang - Quy trinh hieu chuen tam th&i

X-rayfluoresc>nce Spectrometers - Temporary calibration procedure

1. P h ~ m vi a p dgng

VBn bin ky thujt nay qui djnh quy trinh hieu c h u b thiet bj hujllh quang'tia X (XRF) (sau a y poi 18 thikt bj X-Ray) diing dk x b djnh him lupng nguyCn tb kim loai vang (Au) trEn b& mat cac rngu hlrp kim ving trang sirc viri k b th6ng s6 dgc trung i j t h u t nhu sau:

- Pham vi do (Au): (0 + 99,99) %;

- Sai s6: dugc buy djnh theo timg dii do, cy thk nhu sau:

+ Dbi viri ving hlrp kirn c6 him l u p g Au (30 + 99) %: kh6ng nho h m 0,06 %;

+ Dbi v6i vhng hqp kim co him lupng Au 99 % trb 1En: kh6ng nho h m 0,01 %.

2. Cac phep hi@ chuHn

Phai l h lugt ti&n hanh cac phCp hieu chuhn ghi trong bang 1. Bang 1

3. Phvcrng tien hi@ chuHn

Phumg tien hieu chuhn phuc vu viec hi@ chuhn thik bj X-Ray c6 d$c tnmg i j thufit do

l u h g ccr bin duac quy djnh trong bang 2 duai diiy:

1 1 ~i: tra ky thujt

KiEm tra do l u h g

Theo diiu myc c6a quy trinh

6.1

TT

1 1

6.2

6.3

TBn ph6p hieu chukn

~ i & m tra bCn ngoai

TT

1

. .

TBn phumg tien hi@ chukn

1.1

~ h u h n do l u h g

D#c trung @ thu@ do l u h g ccv bin

dyng cho digu myc cua

quy trinh

bqc (Ag) vdhofic ddag (Cu). Dij khBng dim bao do: u 5 0,04 %

Bij chit chudn ving (Au)

dugc chimg nh& trCn n&n

Gia tri him lupng vang (Au) danh

djnh: (30 + 99) %. 6.3

/ I do am mai tnrbng. 1 Gil trj do chia: 1 OC. t I

Gia tri ham luqng ving (Au) danh

djnh: - 99,99 %. 1.2

2

- Do dm kh6ng khi: 1 4 1

De kh6ng dam bao do: u 5 0,005 %

c h i t c h u b vang (Au) tinh

khi6t dugc chimg nh$n.

I I 1 Gil trj do chia: 1 %RH. I I '

Phvcmgtifn khac

I I 1

I Dung djch rira, l h sach b& Dung mdi lam sqch la c8n tuyet 1 1

Phumg tien do nhiet do va

1 2.2 m@t chit c h u b ving, nubc

- Nhiet do: (0 + 50) OC;

I

1 GBng tay, panh gBp chiit

chuin vhng, ao blouse,. . .

4. ~ i k u kien hi@ chuhn

Khi tien h& hieu c h u b phai dam blo c b di&u kien sau diiy:

- Nhiet do: (10 + 30) "C;

- Do hm kh6ng khi : (30 + 80) %RH;

- Khu vuc b6 tri thiit bi c h tranh tac dong bSn ngoai nhu: may phat dien, may han, song dien tu, dien cao ap, . . .

5. ~ h u h n bj hi@ chuhn

Trubc khi ti&n hanh hi& c h u b phai chuin bj cac cdng viec sau diiy:

- Chon t6i thi&u 05 chdt c h u b the0 muc 3 tai cac di&m hi@ chuhn co ham luqng Au danh djnh phiin b6 d&u trong khoang: (30 + 99) % va 01 chit chudn c6 him luqng Au danh djnh 99,99%.

- B$t nguBn thiit bi X-Ray va dB an djnh it nhdt 30 phut truirc khi hieu chuin.

- V$n hlnh thi6t bj the0 ddng h u h g dfh sir dung cha nha san xu& thiet bj X-Ray.

- LBm sqch b$ mgt chit'chuin Au: Tnrirc khi tikn h h h thir nghiem, loqi b6 nhism bin tr@n b$ mat c h k chuin Au bing can tuyet d6i, sau d6 nia lqi v6i nuirc tinh khiikt (nuirc c h 1 lhn) va lam khb b$ mat chit chuin Au.

6 ~ i 6 n h a n h hie" chuHn

6.1 ~ i $ m t ra bCn ngohi 8

- Kikm tra bingomit d& x C dinh sy phii hgp clia thiikt bj X-Ray d6i viri c ic yCu chlu quy djnh trong tai lieu ky thugt, vk hinh d h g , kich thvirc, hiin thj, nguBn dien sir dung, nhZn hi@ va phu kien kem theo.

- Kikm tra trqngjhai hoat d@ng binh thubng clia thikt bj X-Ray the0 tii lieu ky thugt.

6.2 Ki&m t ra kf thugt ( ~ i & m t ra dij tuy&n tinh) (rip dung dbi vc?i cac thi&t bi X-Ray cd khci niing do duqc ccic gici tri niing lugng ri6ng biet cho tkng loai nguy6n tb AU, Ag, Cu,.. )

- Chon c k d9i do (nku c6) quy djnh tr&n thikt bj X-Ray.

- ~ 6 i viri thikt bj X-Ray khbng c6 dir lieu dubng n@i c h u h luu trong p h h mkm tinh toin: hik kt lgp d u h g cong hi& c h u h (calibration curve) tr&n b@ chit chuin vang kem the0 thikt bj X-Ray clia ca sb sir dung v6i t6i thiku 05 chit chuin ving c6 cic gia trj danh djnh xip xi cac gi9 trj danh djnh quy djnh trong muc 5 v i phi^ hqp viri diii do c h hieu chuin tr&n thikt bj X-Ray.

- Thuc hien t6i thiku 5 phep do lidn ti$ viri m8i chk c h u h da chon. Ghi kkt qua do duqc vio bi6n ban 6 phu luc 1.

- He s6 hai quy R~ cua d u h g cong hieu chuin khbng duqc nho han 0,99.

6.3 Ki6m t ra do lubng (Ki&m t ra di) chinh xic)

- Lua chon t6i thiku 05 chit c h u b c6 gia trj danh djnh (theo muc 5) phh hqp v6i dHi do chn hi& c h u h dk ki&m tra d@ chinh xac cua thiikt bi X-Ray chn hi@ chuin.

- ~ i k n hanh do tbi thi$5 phep do lien tikp v6i m8i chih c h u h d5 chon viri cic g i i trj danh djnh l in llogt tu th$ dkn cao. Ghi kkt qua do duqc v b bi6n bin ir phu luc 1.

- Sai s6 tuyet dbi duqc tinh the0 cbng thuc sau: -

A=C, -C,

Trong 86 :

A - Sai s6 t ~ y e t dhi, %;

Cd - Gia tri him luqng Au do duqc, %;

CCh - Gii trj him luqng Au cua chit chuin, %;

6.4 U'&c lwqng di) kh8ng ham bao cua phCp do

6.4.1. Ubc l u p g do khdng d b bao chuin loai A:

- Gia tri trung bi+ cua n phkp do:

- £30 lech c h u b thuc nghiem cua gia tri trung binh: g

- Do khdng dam bao gly nen bbbi dQ phln giai cua thi&t bi c& hi@ c h u b :

~ h i 6 t bi X-ray c h hi& chuhn c6 dQ phln giai (gia tri dQ chia) la a (%)

- Do khdng dam bHo c h u b loai A:

6.4.2. Ubc l u p g 86 khdng dim bao c h u b loai B:

c h i t chuhn v b g co do khBng dam bao do trich d h la b (theo ~ i 6 ~ chimg nhb) , v& k = 2 Y

! 1

va p = 0,95: -. - . ,

. "

6.4.3. U'irc l u p g do khdng d h bao chuPn tdng h w : , < ' .ri

6.4.4. U'trc luqng dij khdng d h bao chuin mb rijng:

U = k.uc

k 1& he s6 ph8 (k = 2 tumg dumg v6i xac suit tin c$y P = 0,95).

, 7. Xiu 19 chung

7.1 ~ h i 8 t bi hujmh quang tia X (XRF) xac djnh ham luqng v h g sau khi dugc hi& chuhn,

n8u dat cac y h u iu quy d b h the0 quy trinh hi& chuhn nay dugc chp c h h g chi hi& chuin

(tem hi@ c h u b , gihy c h h g nhan hi& c h u b , ...) the0 quy djnh kkm the0 thbng bao kkt

qua hi& chuhn.

7.2 Chu kjr hieu c h u b : 01 n5m.

v

Phu lqrc 1

. A Ten thiet bi: ..................................................................................................................... . A ......................................................... ................................................................. Kieu: S8:

Ca s6 s in xuiit: .......................................... Ngm s k xuht: ............................ J ................

. A Phucmg phap thuc hien: ................................................................................................. Ca s6 su dung: ....................................................................................................... ......................................................................................................................................... Di&u kien m6i tnrimg:

. A Nhiet @: ................................................................ h: ............................................. . A Nguiri thuc hien: .............................................................................................................

Ngay thuc hien : ............................................................................................................. ....................................................................................................... Dia di6m thuc hien :

1. Ki&m tra b&n ngoai:

2. Ki6m tra ky thuijt (Ki6m tra dij tuy& tinh):

n. ..........

Ham lugng (%)

PhCp do

1

2

3

4

5

Ch5t chuiin s8

-----

-----

-----

2. 1.

Trung binh:

3.

I

3. ~ i & m tra do l w h g ( ~ i & m tra db chinh xhc):

ChBt c h u h s6

Ham luqng (%)

Phip do

1

2

3 Q

3. 1.

4

. . . . . . . . . .

8

2.

5 .

......

Trung binh :

n.

-

V06.M-17.14 ~ h 8 k& hujmh quang tia X - Phumg ph$ hi& chub.

DLVN 11 3 : 2003 Y&u chu v& nbi dung va cich trinh bay v5in b8n ky thuat Do l u h g Viet Nam.