Rigaku NIC MA-3000 Operating instructions

Troubleshooting FAQs

for

MA-3000

Ver 1.0

MA-3000 Troubleshooting FAQs

Leak Check Fails

Q: Leak Check (Check of flow path) fail

Situation Possible causes to be confirmed

①

、②、④

③、④、⑤、⑥、⑦

(i) NG is generated by any of the V1 to V3 checks.

⑧

、⑨

Possible causes:

①

Dirt in the inlet port

②

Missalignment of MFC

③

Damage to sample heating tube

④ Loose or damaged joints

⑤

Deterioration of O-ring (P22A), installation fail

⑥

V3 valve failure

⑦

Damaged Z-axis nut

⑧

Clogged sample heating tubes and outlet activated carbon filter

⑨

Damage to pressure regulator

①：Dirt in the inlet port　

Recommended action:

a. Turn off MA-3000

b. confirm that the temperature at the inlet port has cooled,

c. check the inlet port and the O-ring.

d. If there is any dirt or foreign matter, wipe it off using paper with ethanol.

②：Misalignment of MFC

Recommended action:

For Old Type of MFC (Blue)

a. Check on the maintenance screen, visual check:

b. Remove the right side plate/cover of MA-3000

c. Adjust with the trimmer for origin adjustment (Picture 1) with no flow.

(i) Flow rate value does not drop from 0.01 to 0.02 L/min.

(ii) Flow rate value does not drop from 0.2 to 0.4 L/min.

Answer 1: If the leak check fails with NG, the following

situations are possible:

Answer 2 : If the plumbing check fails with NG, the

following causes is possible:

Picture 1

MA-3000 Troubleshooting FAQs

For New Type of MFC (Silver)

a. Check on the maintenance screen, visual check

b. Remove the right side plate/cover of MA-3000

c. Press and hold small button (Picture 2) with no flow rate.

③：Damage to sample heating tube

Recommended action:

a.Visual check: life of sample heating tube,

c. Check for swelling signs or damage due to moisture absorption.

d. Replace a new sample heating tube if sample heating tube damage is found

④：Loose or damaged joints

Recommended action:

b. Check if there is any measurement of samples that could react with quartz such as fluorine

which shorten sample heating tube lifespan

a. Check by hand tightening: Turn it lightly in the loosening direction, and if it turns easily,

retightens it.

b. Tighten the different-diameter joints lightly by hand and then retighten about 1/2 turn with a

wrench.

c. Check by hand tightening: The screw idles when tightened and/or nut section is bent at an

angle, the screw section may be damaged. Replace a new one. (Picture 3)

Picture 2

Picture 3

MA-3000 Troubleshooting FAQs

⑤

：Deterioration of O-ring (P22A), installation fail

Recommended action:

Check O-ring from the port side whether O-ring slipping off or broken.

⑥：V3 valve failure

Recommended action:

b. if the leak check passes, the Tygon tubemust be replaced.

⑦：Damaged Z-axis nut

Recommended action:

a. Take out Z-axis nut from Z-axis assembly and check if it is damaged.

b. If it is damaged, replace a new one.

⑧：Clogged sample heating tubes and outlet activated carbon filter

Recommended action:

a. Check by replacing parts.

Note: Periodic replacement (1-year replacement) of activated carbon filter is strongly recommended.

⑨：Damage to pressure regulator

Recommended action:

Note: Put back the Tygon tube after at least 5 seconds after conditioning starts. Otherwise the catalyst in

sample heating tube may shift

If the activated carbon filter is not replaced for a long period of time, it will cause in decrease of

mercury removal rate and hence, NG in the check of flow path.

Check the pressure regulator on the rear panel and replace it if the gauge exceeded maximum

value.

a. Check during leak check: Remove the right side plate/cover of MA-3000, start leak check, and

bend the Tygon tube as shown in Picture 4,

Picture 4

MA-3000 Troubleshooting FAQs

Contamination

A: This situation is most likely due to severe contamination.

Depending on the frequency and concentration, please follow the steps below for repair.

①

　Repeat "Purge" measurement

②

　Wash joints

③

　If there is no improvement after the steps

①

and

②

④

　If there is no improvement after the step

③

①：Repeat "Purge" measurement

a. Prepare several sample boats with 200 µl of water and

b. Repeat the measurement by alternating water and purge measurement in the sample tab.

c. This will gradually remove the mercury residue and decrease the blank.

d. Check the blank again after repeating several measurements.

②：Wash joints

a. Wash joints and cells (refer to instruction manual).

b. Perform

①

again after assembling the cleaned parts.

③：If there is no improvement after the operations in ① and ②

b. After that, perform step

①

④：If there is no improvement after the operation ③

Q: What should I do if a cell dark error occurs after sample measurements?

If mercury remains in the cell or in the tubing, it will later wriggle out and cause cell dark.

Recommended action:

When this happens, perform purge sufficiently and repeatedly. If contamination persists, parts

may need to be replaced.

Q: After measurement of sample with high mercury concentration, the blanks do not go

down. What should I do?

a. Replace the "boat handling poker," "sample heating tube," and "collector tube" according to

the instruction manual.

a. Other parts (solenoid valves, gas-liquid separation pipes, feed ports, and piping for each

section) and activated carbon filters need to be replaced.

b. If there is no improvement after performing the operations described in

②

④

, please

contact NIC for further assistance.

A: Cell dark error is most likely triggered by system contamination due to excessive amount of

mercury released from sample after thermal decomposition.

MA-3000 Troubleshooting FAQs

Q:Sensitivity is low, what should I do?

Phenomena of low sensitivity includes:

1. Poor recovery of check standards

2. Poor recovery of CRM/SRM measurement

A: Below are possible causes:

Standards Solution related:

①Deterioration of standard solutions or standards preparation errors

Sample Nature related/Application issue:

②Decreased sensitivity due to sample nature

Consumables and hardwares/parts related:

③

Lifespan of sample heating tube/combustion tube

④Contamination of tubing, joints

⑤Accumulated dirt on sample boat

External factors:

⑥Affected by environment

Recommended action:

Possible Cause ②：Decreased sensitivity due to sample nature

Recommended action:

Possible Cause

①

：Deterioration of standard solutions or standards preparation

errors

- For heating method, prepare a standard solution using 100 ppm of L-cysteine solution in the

diluent.

- For reducing vaporization, prepare a standard solution using 10 ppm of L-cysteine solution

in the diluent.

Some sample types (such as sample contains high level of halogen, sulphur or oil) may

cause decreased sensitivity of the instrument after sample measurement. For samples with

poor reproducibility, measure the standard solution after the measurement to confirm.

If a decrease in sensitivity is occurring, it is necessary to change the measurement method,

reduce the sample volume, use an additive, or otherwise change the measurement technique.

Low Sensitivity

Mercury standard solutions are unstable, it can be easily adsorbed onto the glassware

surface or volatilized causing lost of mercury analyte.

a. To avoid mercury memory effect on the glassware, all glasswares used in the preparation

of mercury standard solutions should be thoroughly washed with 10% nitric acid.

b. We also recommend the use of L-cysteine solution in the diluent to provide better retention

of mercury.

Note: Please consult NIC for application advice if sample gives poor reproducibility or causes poor

sensitivity after measurement.

MA-3000 Troubleshooting FAQs

Possible Cause

③

：Lifespan of sample heating tube

Recommended action:

a. If the number of measurements is more than 2000 times, please replace it.

Possible Cause ④：Contamination of tubing, joints

Recommended action:

Tubing will need to be replaced, fittings cleaned, etc.

Possible Cause ⑤：Accumulated dirt on sample boat

In the case where:

Recommended action:

⑥：Affected by evironment

Instrument is located in a room/environment consists of some interfering compounds

Recommended action:

Never use/operate instruments in rooms consists of halogenated reagents such as

organochlorine solvents or potassium iodide.

・If the tubing is contaminated, or if the gold in the collection tube section is blown into the

piping at the latter stage, a decrease in sensitivity may occur.

- there is no separation of boats used for mercury standard solution and sample

measurements;

- and after measurement, these sample boats are only heat treated without washing for a

long period of time,

In rare cases, reducing substances may accumulate within the sample boat which decreases

instrument sensitivity over time.

Soak and wash the sample boats in 1% nitric acid for 8 hours or more may improve the

situation.

If usage of sample heating tube has exceeded its lifespan (typically 2000 times), the internal

catalyst will no longer be able to remove interfering components effectively, and thus it

affects the system's sensitivity, optimum performance cannot be achieved.

b. If the number of measurements is less than 2000 times, repeat the purge and 200 μl of

water for 5 sets of measurements to see if the sensitivity recovers.

MA-3000 Troubleshooting FAQs

Troubleshooting in Optional Attachment - SCRD

Q: Sensitivity error occurs with optional units (SC-3+RD-3, SC5+RD5).

A: Below are the possible causes of poor sensitivity:

① Flow rates are decreasing.

② There is leak.

③ Sample tube is contaminated.

①：Flow rates are decreasing.

・Replace the air pump tube if the replacement frequency (1 year) is exceeded.

・Visually inspect the air pump rotor and replace it if it is shaved or dented (Picture).

・Visually check the membrane filter and replace it if it has water droplets on it.

②：There is leak.

b. If MA-3000 standalone passes leak check, setup the configulation back to SC/RD.

d. If the bubbling is weaker than usual (less bubbles observed), check ① again.

③：Sample tube is contaminated.

a. Dispose of the measurement effluent in the sample tube.

Remark:

- Always perform alkaline rinsing of the sample container after each measurement.

- If you do not have an ultrasonic cleaner, soak the container overnight and scrub it with a brush.

- If alkaline detergent is not available, a 0.1M sodium hydroxide solution will also work.

④ Problems specific to reducing vaporization (blanks, standard solution, pretreatment, etc.)

- Do not mix measurement effluent with heavy metal solutions or other liquids that may

contain mercury.

b. After rinsing with water, place in a container with alkaline detergent solution and

ultrasonically clean for 30 minutes.

- If SnCl 2 remains in the sample container, it will react with mercury and volatilize while waiting for

measurement.

a. From System→Setup, set SC/RD to None (NONE) and confirm that the MA-3 alone

passes the leak check.

c. Fill the sample tube with about 5 mL of water and perform the measurement to confirm

bubbling.

- This step is important to eliminate the contamination issue because alkaline detergent solution can

remove SnCl2 effectively.

MA-3000 Troubleshooting FAQs

d. After further rinsing with water, rinse with distilled water.

e. Dry and store to prevent dust, etc. from entering.

Please check the FAQs for the reduction vaporizer (RA-4500).

The standard solution may deteriorate, the L-cysteine concentration may be wrong, the

sensitivity may decrease during pretreatment, or the blank may rise during pretreatment.

c. Next, rinse well with water and ultrasonically clean in the same way with nitric acid (1+10)

for 30 minutes.

Remark: If cleaning detergent or nitric acid is used repeatedly, it may be contaminated. Please

replace it with a new one periodically.

- If you use a dryer after washing, please refrain from using it once as there is a possibility of

contamination during drying.

Remark: Sample tube that are opaque or have noticeable scratches will be difficult to clean. Replace

it with a new one.

④

：Problems specific to reducing vaporization (blanks, standard solution,

pretreatment, etc.)

MA-3000 Troubleshooting FAQs

Troubleshooting in Optional Attachment - RH-MA3

Q:Sensitivity error occurs in the optional unit (RH-MA3).

A: Below are the possible causes :

①

Flow rates are decreasing.

②

There is leak.

③

Tube is contaminated.

④

Collector tube is degraded.

①　Flow rates are decreasing.

b. Replace the air pump tube if the replacement frequency (1 year) is exceeded.

c. Visually inspect the air pump rotor and replace it if it is shaved or dented.

②　There is leak.

a. Drain the buffer solution completely.

b. Tighten the roller clamps x2 if they are loose. If the silicone tube is damaged, replace it.

d. Setup configulation back to RH-MA3

g. After checking, slowly remove your finger from the collector tube.

Note:

Please be careful not to remove your finger from the collector tube too abruptly.

It may cause the gold component or quartz wool in collector tube to shift.

③：Tube is contaminated.

b. If gold or dirt from the collection tube adheres to the downstream,

④：Collector tube is degraded.

Recommended Action:

The collection tube is a consumable item, and periodic replacement is recommended.

a. Fill the wash bottle with distilled water, perform the measurement, and check for bubbling.

a. Contamination of the MA-3000 V4 valve and RH-MA3 tubing may result in poor data.

Please replace them periodically (about once/year).

- Clean the wash bottle, dehumidifying bottle, and fittings using 1+10 nitric acid and ultrasonic

cleaning for 30 minutes or soaking for at least 8 hours.

- If cleaning of parts does not restore the system, replace the above parts (air rinse bottle,

dehumidification bottle, and fittings) and piping tubes with new ones.

If the quartz wool at the rear of the collection tube is discolored, or if the collector is not fixed

in place and has shifted, mercury leaks during sampling and gold may jump to the latter stage,

resulting in reduced sensitivity.

c. From System→Setup, set SC/RD to None (NONE) and confirm that the MA-3 alone passes

the leak check.

e. With the buffer solution completely drained, connect the collection tube and start

measurement, then press down the inlet of the collection tube with your finger.

f. If air can be removed from the silicone tube at the bottom of the air wash bottle, there is no

leak.

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