dma-80 testing procedure

4
This brief procedure has been intended as a Service tool to be followed everytime you meet analytical issues on the DMA80 instruments and for the which you find difficult the resolution. Fill in and follow the procedure step by step. General information Company Person in charge Testing date Technical data Unit Serial Number: Terminal type or USB-640 Gateway: SN: Software, type and revision: Rev.: Gas carrier Oxygen Air Compressor Purity: SN: Gas system pump (if present) SN: Catalyst tube LOT: Inst. on: Amalgamator tube LOT: Inst. on: Installation and last maintenance dates: Inst. on: Maint. on: DMA-80 Hardware information Internal pressure bar: Flow rate l/h: Amalgamator stand by temperature °C: Amalgamator heating temperature °C: Catalyst temperature °C: Cuvette temperature °C: Drying decomposition temperature °C: OFFSET detector VDC: GAIN detector VDC: Milestone Srl – Via Fatebenefratelli 1/5 – 24010 Sorisole (BG) Italy Phone: 0039-035-573857 – Fax: 0039-035-575498 – e.mail: [email protected] Page 1/4 TECHNICAL NOTE Subject: DMA-80 Testing procedure Ref. Model(s): DMA-80

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Page 1: DMA-80 Testing Procedure

This brief procedure has been intended as a Service tool to be followed everytime you meet analytical issues on the DMA80 instruments and for the which you find difficult the resolution. Fill in and follow the procedure step by step.

General informationCompany

Person in charge

Testing date

Technical dataUnit Serial Number:

Terminal type or USB-640 Gateway: SN:

Software, type and revision: Rev.:

Gas carrierOxygen Air Compressor

Purity: SN:

Gas system pump (if present) SN:

Catalyst tube LOT: Inst. on:

Amalgamator tube LOT: Inst. on:

Installation and last maintenance dates:

Inst. on: Maint. on:

DMA-80 Hardware information

Internal pressure bar:

Flow rate l/h:

Amalgamator stand by temperature °C:

Amalgamator heating temperature °C:

Catalyst temperature °C:

Cuvette temperature °C:

Drying decomposition temperature °C:

OFFSET detector VDC:

GAIN detector VDC:

Milestone Srl – Via Fatebenefratelli 1/5 – 24010 Sorisole (BG) ItalyPhone: 0039-035-573857 – Fax: 0039-035-575498 – e.mail: [email protected]

Page 1/3

TECHNICAL NOTE

Subject:

DMA-80 Testing procedure

Ref. Model(s):DMA-80

Page 2: DMA-80 Testing Procedure

Testing procedure

1. Initialize the consumables: run the procedure here below in order to remove humidity and each trace of contamination from the consumables

StepReagent/sample

type

Sample

amount

DMA80 program

Drying time and temp.(1) (2)

Decomposition time and temp.(1) (2)

Purge/waiting time

1°-2° B/V amalgamator - - - -

3°-4°-5°Blank

(without sample boat)

100mg (indicat

ive value)

IR: 10sec/300°C + 120sec/300°C

IR: 60sec/850°C + 120sec/850°C

70secATC: 10sec/200°C + 120sec/200°C

ATC: 60sec/650°C + 120sec/650°C

6°Common white flour

+ distilled H2O300mg+50mg

IR: 10sec/300°C + 120sec/300°C

IR: 60sec/850°C + 120sec/850°C

70secATC: 10sec/200°C + 120sec/200°C

ATC: 60sec/650°C + 120sec/650°C

7°-8°Blank

(without sample boat)

100mg (indicat

ive value)

IR: 10sec/300°C + 120sec/300°C

IR: 60sec/850°C + 120sec/850°C

70secATC: 10sec/200°C + 120sec/200°C

ATC: 60sec/650°C + 120sec/650°C

9°Common white flour

+ distilled H2O300mg+50mg

IR: 10sec/300°C + 120sec/300°C

IR: 60sec/850°C + 120sec/850°C

70secATC: 10sec/200°C + 120sec/200°C

ATC: 60sec/650°C + 120sec/650°C

10°Blank

(without sample boat)

100mg (indicat

ive value)

IR: 10sec/300°C + 120sec/300°C

IR: 60sec/850°C + 120sec/850°C

70secATC: 10sec/200°C + 120sec/200°C

ATC: 60sec/650°C + 120sec/650°C

(1) The program has to be set according to the type of temperature control on the Drying/Decomposition furnace: external infrared (IR) or internal thermocouple (ATC) sensor.(2) In case of T640-660/T1640-1660 controller the reported temperature and time refer to the “holding” step(3) Quartz sample boat required. In case of metal boats usage, they must be deeply cleaned before to run a stability test.

2. After conditioning, two stability tests are required:

Stability of 100µl of 100ppb (10ng)

a) Run minimum 2 blanks on the same sample boat (quartz if possible) in manner to clean itb) Run blanks until absorbance value (Height) decrease under 0.0020c) Set a fresh and stabilized 100µg/L Hg standard according to the prescriptions reported on the

DMA80 User Manual. The quality of the used standard is fundamental for the success of the entire procedure

d) Weight approximately 100µg of the fresh 100µg/L – Standard (10ng) and start the analysis as a single measurement mode

e) Repeat five times the testf) Run again two blanks measurements

Stability of 500 µl of 100ppb (50ng)a) Run minimum 2 blanks on the same sample boat (quartz if possible) in manner to clean itb) Run blanks until absorbance value (Height) decrease under 0.0020c) Set a fresh and stabilized 100µg/L Hg standard according to the prescriptions reported on the

DMA80 User Manual. The quality of the used standard is fundamental for the success of the entire procedure

d) Weight approximately 500µg of the fresh 100µg/L – Standard (10ng) and start the analysis as a single measurement mode

e) Repeat five times the testMilestone Srl – Via Fatebenefratelli 1/5 – 24010 Sorisole (BG) Italy

Phone: 0039-035-573857 – Fax: 0039-035-575498 – e.mail: [email protected] 2/3

TECHNICAL NOTE

Subject:

DMA-80 Testing procedure

Ref. Model(s):DMA-80

Page 3: DMA-80 Testing Procedure

f) Run again two blanks measurements

Evaluation of the results and temperature adjustmentUnit properly working

Stability of 100µl of 100ppb (10ng) Stability of 500 µl of 100ppb (50ng)

RSD ≤ 3%Absorbance range: from 0.4200 to 0.5700

RSD ≤ 3%Absorbance range (cell 2) from 0.0400 to 0.0600

If the results do not pass the above acceptance criteria or/and they show the following issues:- first reading of the stability very low- low absorbance- big difference of Hg concentration from the test with 10ng compared with the test with 50ng

Send the document filled in and the measurement file in .d80 format to Milestone s.r.l. at [email protected] for evaluation.

Milestone Srl – Via Fatebenefratelli 1/5 – 24010 Sorisole (BG) ItalyPhone: 0039-035-573857 – Fax: 0039-035-575498 – e.mail: [email protected]

Page 3/3

TECHNICAL NOTE

Subject:

DMA-80 Testing procedure

Ref. Model(s):DMA-80

POINT A-B

POINT D-E

POINT F

SINGLE MODE