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MERCURY/MA-3000

Simplified Operation manual

NIC-600-2233-01

Nippon Instruments Corporation

NIC-600-2233-01

1. Preparation
(1). Open the main valve of the Oxygen gas cylinder
and adjust the pressure to 0.10.5Mpa.
(2). Adjust the regulator pressure to 0.05Mpa on the
backside of MA-3.

(3). Confirm whether the drain water is overflowing


from the drain tank.

2. Start-up
(1). Start-up Windows and boot win by clicking

on the desktop.

(2). Turn on the main switch of MA-3000.


(3). Check of flow path screen pop up after initialization.
Click Yes .
Then, the checking of a flow rate, leak, and valve operation is
started.

A message will be displayed if abnormal condition is observed. Software will be terminated


when OK is clicked. Turn off MA-3000 and then fixing them.

(4). After the check is completed, heat - conditioning start.


(H3 is heated for 10 minutes, with flowing.)
(5). It will be in ready state in 20 minutes. Please check that the warning message is not displayed.

3. Decreasing the system blanks


Click

and perform the blank measurements at least three times until getting stable. Or set

SAMPLE_No. 0 registers with a tabulation screen and measures.


(The mercury which remained in the system comes out in the first several measurements when
MA-3000 starts.)

Click to add check on MEAS, and input 0 into SAMPLE_No.


Click

or press F5 to start.

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NIC-600-2233-01

Pretreatment of sample boat


Sample boats absorb mercury in the air and a blank becomes high. In order to measure with
sufficient accuracy, heat-treat to remove mercury sample boats before measurement.
The way of heat-treatment
(a) Sample boats are repeatedly and measured on MA-3000 to confirm low enough.
(b) Sample boats are put into a ceramic crucible, which is heated at 750 for 1 hour or more.

4. Setting for Measurement Condition


() Click

and Measurement Condition is displayed.


Select the proper method for STD. The default
method is already set for standard solution, but
selects the proper method for using SRM (Standard
Reference Materials).
Select Flow rate.
0.1L /min: High sensitivity
(1pg~10ng)
0.2L/min: usual
0.5L/min: high concentration
(Linear range up to 10,000ng)

Enter the proper values in each item of STD Check.

In thermal decomposition mercury analyzing, approx


1% of the prior measured value is detected as a
carryover. If a low-concentration sample is measured
after a high concentration sample, it will be affected
with previous carryover.
Blank Check function provides to automatically lower
a blank.

Typical value (0.2L/min)


ABS(LOW)

ABS(HIGH)

0.1ng

0.002

10ng

0.001

1ng

0.02

100ng

0.01

5ng

0.1

1,000ng

0.1

10ng

0.2

5,000ng

0.4

20ng

0.3

10,000ng

0.6

Please refer this table which number should be


entered.

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5. Setting for Table Condition


Click

and Table Condition is displayed. Select each item of measuring conditions.


Peak/Area
Usually, select Area.
But select PEAK when a peak is small
and AREA value varies.
Solid or Liquid
Select a sample feature. This is not
related to Measuring method.

Calibration curve
y=ax+blank is recommended when
measuring the sample near blank.

6. Measurements
6.1. Registration of standard
Click the tab of "STD.

(1) Click STD to open the STD INPUT box.


Enter the concentration of the
standard solution and the amount
of sample.

(2) Check the Measurement box to add a check


mark to it.
Inject standard solution is put into each sample boat.

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6.2. Starting a measurement


Click

or press F5, and the measuring starts.

At the start, set the file name to save the


measurement data.

6.3. Reviewing a calibration curve


Press icon to switch the Analyze screen to review the Calibration curve.
 Click the
screen.

icon and switch to the Analyze

 Review the calibration curve in CALIB tab.


* When some abnormalities are observed on a
calibration curve, all values of the calibration
become red and "WARNING" is displayed.
 Confirm the calibration curves of LOW and HIGH,
and reject the abnormal data by marking in
box.

Each

instrument

has

its

own

characteristics and differs on sensitivity.


Please refer the optimum sensitivity and
inspection data before shipping.

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6.4. How to mount the samples


Sample amount is depending on the sample kind, form, but 200mg for solid and 200uL for liquid are usually
recommended. Be careful not to be spilled out of the boats during loading in the sample changer.
Wear the gloves or use the tweezers, when weighing samples and handling sample boats.
If the liquid samples may contain organic mercury, add additive B or L-cysteine solution not to
vaporize during standby in the sample changer. Add small amount of additive B in the boat bottom
or add 10uL of 100ppm L-cycteine solution.

When you use additive B, please put small amount of additive into sample boat before sample
weighting.

The volatile high liquid


Add more additive the level of liquid samples
.

The sample which melt after measurement


(Ex. Aluminum, Pyrex and so on)
Put additive at the bottom.

The sample which burns rapidly


Put additive at the bottom on the boat. And put sample
several points on additive, and then cover it with another
additive.

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6.5. Measurement of Unknown samples


(1) Enter the sample name and the sample amount. Select the sample form and unit etc on the
Table Condition by clicking

(2) Select the heating method in Method Number. If the moisture content is known as for solid
samples, enter it in MOIST [%] so that the concentration is calculated as dry weight.
(3) After checking Sample Number with

, click

or press F5 to start measuring.

Selection for (Heating) Method


Select a heating method (12 Methods) can be registered in Run - Method set as Heating Method.
5 Methods are installed by default as described below.
Heating Method table
Method
Kind of sample
No,
Liquid sample /Standard solution
0
Liquid sample with additive B
Biological sample (Solid)
1
Fish tissue, plant tissue
2
Soil, sediment & sludge
3
Urine, Blood
4
Plastics
5

Minerals
Coal, coal ash, metal and mineral

6
7

Waste water
Purge

Heating Method
STD

Typical
amount
~200L

ORGANISM
(SOLID)
SOIL & SLUDGE
URINE & BLOOD
PLASTICS

~200 mg
~200L
~100 mg

MINERAL

~200 mg

WASTE WATER
PURGE

~100L
-

~200 mg

Do not measure the sample digested by HNO3 directly. This sample may generate heat on the
activated carbon filter. Dilute it less than 5wt% of HNO3.
As for HCL solution, dilute it less than 1wt%.
The above Heating Methods may not cover the samples which contain a lot of halogens or burn
quickly.
When the check standard after measuring is lower, reduce the sample size.
Dilute or reduce the sample size if it contains high mercury. Otherwise it contaminates the
plumbing.
As for the liquid samples containing organic mercury, use Additive B on the boat.

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6.6. Starting a measurement


Click the

icon or press F5 to start measuring.

6.7. Reviewing measurement data


Review the measurement results and determine whether to use the data or not.

As for the analysis range, the data less than 10ng are applied for LOW range and the data greater than
10ng are applied for HIGH range. An analysis range can be changed and is performed in the Range
column.
If the recovery of the standard solution after the measurement is 90% or less, it might be due to the
interference contamination. Try to reduce the amount of sample or to change the heating conditions.
Inject 200L of Distilled Water for several times, if high concentration samples are measured.
Inject 200L of Standard Solution repeatedly, if the sensitivity reduces. This way recover the
sensitivity and can also confirm.

7. Data Save
() Press

and Save screen is displayed.

() Select the registered folder and save it with entering the file name.

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8. Printing
() Press

() Select the printing objects and click Print Review.


() Confirm Print Review and start printing.

Select Table-Memo Set


The title and a measurement person name can be inputted on the screen.

The printing profile's scale is being interlocked with the scale of Profile screen. Set up the scale and
the number of profiles of each range by STD and SMP, respectively.
HIGH

Low

Number
of profile

The row width of printing is being interlocked with a setup of Table screen. If the row width at the time
of printing is narrow, please adjust on the screen. And, the row will not be printed if width of a row is
made into zero.

9. Termination
() Press the upper right button

of MA3win.

() Close the Windows and turn off the power of PC and Printer.
() Power off MA-3000.
() Discharge liquid of a drain tank.
() Close the main cock of the Oxygen gas cylinder.

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9 Errors and warning


Measurement can continue even if a warning message has been displayed. However, if an error
message is displayed, measurement will be disabled until the cause of the error has been solved.

Please check messages and contact our service.

Technical Center
14-8 Akaoji-cho, Takatsuki-shi, Osaka 569-1146
Japan
Phone: +81-72-693-6820
Fax: +81-72-694-0663

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